Small-scale synthesis of laboratory reagents: with reaction modeling
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| Main Author: | |
|---|---|
| Format: | Book |
| Language: | English |
| Published: |
Boca Raton [u.a.]
CRC Press
2011
|
| Subjects: | |
| Online Access: | Inhaltsverzeichnis |
| Item Description: | Includes bibliographical references and index |
| Physical Description: | XV, 217 S. Ill., graph. Darst. |
| ISBN: | 9781439813126 |
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MARC
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| 100 | 1 | |a Lerner, Leonid |e Verfasser |4 aut | |
| 245 | 1 | 0 | |a Small-scale synthesis of laboratory reagents |b with reaction modeling |c Leonid Lerner |
| 264 | 1 | |a Boca Raton [u.a.] |b CRC Press |c 2011 | |
| 300 | |a XV, 217 S. |b Ill., graph. Darst. | ||
| 336 | |b txt |2 rdacontent | ||
| 337 | |b n |2 rdamedia | ||
| 338 | |b nc |2 rdacarrier | ||
| 500 | |a Includes bibliographical references and index | ||
| 650 | 4 | |a Chemie | |
| 650 | 4 | |a Chemical tests and reagents |x Synthesis | |
| 650 | 7 | |a SCIENCE / Chemistry / Industrial & Technical |2 bisacsh | |
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Record in the Search Index
| _version_ | 1804145669323096064 |
|---|---|
| adam_text | Contents
Preface
.......................................................................................................................xi
About the Author
.....................................................................................................xv
Chapter
1
Safety in the Laboratory
.......................................................................1
1.1
Introduction
...............................................................................1
1.2
Characteristics of Hazardous Substances Prepared
in This Book
..............................................................................2
1.2.1
Sodium
.........................................................................2
1.2.2
Potassium
......................................................................4
1.2.3
Lithium
.........................................................................5
1.2.4
Cesium
..........................................................................6
1.2.5
Lithium and Sodium Hydrides
.....................................6
1.2.6
Aluminum Bromide
.....................................................6
1.2.7
Lithium Aluminum Hydride
........................................7
1.2.8
Diethylaluminum Bromide and
Triethylaluminum
.........................................................7
1.2.9
Hydrazine Hydrate
.......................................................7
1.2.10
Azides
...........................................................................8
1.2.11
n-Butyllithium 2M in
Hexane
......................................8
1.2.12
Potassium Hydride
.......................................................8
1.2.13
Carbon Disulfide
..........................................................8
1.2.14
Hydrogen
Sulfide
..........................................................9
1.2.15
Carbon
Tetrachloride
and Chloroform
.........................9
1.2.16
Triphosgene
..................................................................9
1.2.17
Phosphorus Trichloride, Oxychloride, and
Pentachloride
..............................................................10
1.2.18
Sulfur Trioxide and Oleum
........................................10
1.2.19
Thionyl Chloride
........................................................11
1.2.20
Sulfur Chlorides
.........................................................11
1.2.21
Chlorosulfonic Acid and Pyrosulfuryl Chloride
........12
Reference
............................................................................................12
Chapter
2
Sodium
...............................................................................................13
Summary
............................................................................................13
Applications
.......................................................................................13
2.1
Introduction
.............................................................................13
2.2
Discussion
................................................................................14
2.2.1
Basics of Cell Operation
.............................................14
2.2.2
Cell Regimes
..............................................................15
Contents
2.2.3
Cell Equation
..............................................................18
2.2.3.1
Preliminaries
..............................................18
2.2.3.2
Relation between Drop Volume and
Surface Area
...............................................19
2.2.3.3
Deriving the Cell Equation
.........................20
2.2.4
Thermal Balance
........................................................24
2.2.5
Time Required for Melting
........................................25
2.2.6
Cell Corrosion
............................................................26
2.3
Experimental
...........................................................................26
2.3.1
Introduction
................................................................26
2.3.2
Setup and Operation
...................................................27
References
..........................................................................................30
Chapters Potassium
............................................................................................33
Summary
............................................................................................33
Applications
.......................................................................................33
3.1
Introduction
.............................................................................33
3.2
Discussion
................................................................................35
3.2.1
Cell Equation
..............................................................35
3.2.1.1
Preliminaries
..............................................35
3.2.1.2
Deriving the Cell Equation
.........................40
3.2.1.3
Experimental Confirmation of the
Cell Equation
..............................................42
3.2.2
Cell Regime
................................................................43
3.2.3
Cell Corrosion
............................................................44
3.3
Experimental
...........................................................................45
References
..........................................................................................48
Chapter
4
Lithium
...............................................................................................51
Summary
............................................................................................51
Applications
.......................................................................................51
4.1
Introduction
.............................................................................51
4.2
Discussion
................................................................................53
4.3
Experimental
...........................................................................55
References
..........................................................................................58
Chapters Cesium
................................................................................................59
Summary
............................................................................................59
Applications
.......................................................................................59
5.1
Introduction
.............................................................................59
5.2
Discussion
................................................................................61
5.3
Experimental
...........................................................................65
References
..........................................................................................68
Contents
Chapter
6 Lithium Hydride
and Sodium
Hydride...............................................71
Summary
............................................................................................71
Applications.......................................................................................71
6.1
Introduction
.............................................................................71
6.2
Discussion................................................................................
73
6.2.1
Hydrogénation
of Sodium at Atmospheric
Pressure
......................................................................74
6.3
Experimental
...........................................................................77
6.3.1
Sodium Hydride
.........................................................77
6.3.2
Lithium Hydride
.........................................................78
References
..........................................................................................79
Chapter
7
Bromine
..............................................................................................81
Summary
............................................................................................81
Applications
.......................................................................................81
7.1
Introduction
.............................................................................81
7.2
Experimental
...........................................................................82
References
..........................................................................................84
Chapterå
Aluminum Bromide
...........................................................................85
Summary
............................................................................................85
Applications
.......................................................................................85
8.1
Introduction
.............................................................................85
8.2
Experimental
...........................................................................86
References
..........................................................................................88
Chapter
9
Lithium Aluminum Hydride
..............................................................89
Summary
............................................................................................89
Applications
.......................................................................................89
9.1
Introduction
.............................................................................89
9.2
Discussion
................................................................................91
9.3
Experimental
...........................................................................91
9.3.1
Lithium Aluminum Hydride
......................................91
9.3.2
Reduction of Benzonitrile with LiAlH4
.....................94
9.3.3
Calcium Aluminum Hydride
......................................95
References
..........................................................................................95
Chapter
10
Triethylaluminum and Diethylaluminum Bromide
............................97
Summary
............................................................................................97
Applications
.......................................................................................97
10.1
Introduction
.............................................................................97
10.2
Discussion
................................................................................98
viii Contents
10.3
Experimental
.........................................................................100
10.3.1
Ethyl Bromide
..........................................................100
10.3.2
Magnalium
...............................................................101
10.3.3
Diethylaluminum Bromide
.......................................101
10.3.4
Triethylaluminum
.....................................................103
10.3.5
Diethylaluminum Bromide
from Ethylaluminum
Sesquibromide
..........................................................105
References
........................................................................................106
Chapter
11
Hydrazine
Sulfate
and Alcoholic Hydrazine Hydrate
......................107
Summary
..........................................................................................107
Applications
.....................................................................................107
11.1
Introduction
...........................................................................107
11.2
Discussion
..............................................................................108
11.2.1
Hydrazine
Sulfate
.....................................................108
11.2.2
Hydrazine Hydrate
...................................................110
11.2.3
Hypochlorite
Titration
with Iodine
..........................
Ill
11.2.4
Hydrazine
Titration
with Iodine
...............................
Ill
11.3
Experimental
.........................................................................112
11.3.1
Hydrazine
Sulfate.....................................................112
11.3.2
Hydrazine Hydrate in Alcohol
.................................114
11.3.2.1
Using
КОН
............................................... 114
11.3.2.2
Using NaOH
..............................................114
References
........................................................................................114
Chapter
12
Sodium and Potassium Azide
...........................................................117
Summary
..........................................................................................117
Applications
.....................................................................................117
12.1
Introduction
........................................................................... 117
12.2
Discussion
..............................................................................117
12.3
Experimental
.........................................................................119
12.3.1
Isopropyl Nitrite
.......................................................119
12.3.2
Potassium Azide
.......................................................120
12.3.3
Sodium Azide
...........................................................121
References
........................................................................................121
Chapter
13
Potassium r-Butoxide and Potassium Hydride
.................................123
Summary
..........................................................................................123
Applications
.....................................................................................123
13.1
Introduction
...........................................................................124
13.2
Discussion
..............................................................................125
13.2.1
The RLi-TMEDA Complex
.....................................125
13.2.2
Schlosser s
Superbase
...............................................126
Contents ix
13.3
Experimental
.........................................................................127
13.3.1
Potassium
ř-Butoxide
................................................127
13.3.2
Potassium
Hydride...................................................128
13.3.3
Lithium
Hydride.......................................................130
References
........................................................................................131
Chapter
14
Carbon Disulfide
..............................................................................133
Summary
..........................................................................................133
Applications
.....................................................................................133
14.1
Introduction
...........................................................................133
14.2
Discussion
..............................................................................134
14.3
Experimental
.........................................................................136
References
........................................................................................139
Chapter
15
Chlorine
............................................................................................141
Summary
..........................................................................................141
Applications
.....................................................................................141
15.1
Introduction
...........................................................................141
15.2
Experimental
.........................................................................142
References
........................................................................................142
Chapter
16
Carbon
Tetrachloride........................................................................145
Summary
..........................................................................................145
Applications
.....................................................................................145
16.1
Introduction
...........................................................................146
16.2
Discussion
..............................................................................146
16.2.1
The Photolytic Efficiency
.........................................149
16.2.2
Comparison with Experiment
..................................151
16.3
Experimental
.........................................................................151
References
........................................................................................154
Chapter
17 ßfs-Trichloromethyl
Carbonate (Triphosgene)
.................................157
Summary
..........................................................................................157
Applications
.....................................................................................157
17.1
Introduction
...........................................................................157
17.2
Discussion
..............................................................................158
17.3
Experimental
.........................................................................160
References
........................................................................................162
Chapter
18
Phosphorus Pentachloride
................................................................163
Summary
..........................................................................................163
Applications
.....................................................................................163
18.1
Introduction
...........................................................................163
18.2
Discussion
..............................................................................164
x
Contents
18.3
Experimental
.........................................................................165
References
........................................................................................167
Chapter
19
Phosphorus Oxychloride
..................................................................169
Summary
..........................................................................................169
Applications
.....................................................................................169
19.1
Introduction
...........................................................................170
19.2
Discussion
..............................................................................171
19.2.1
Reaction between P2O5 and NaCl
............................171
19.2.2
Reaction between Ca3(PO4)2, Carbon,
and Chlorine
.............................................................171
19.3
Experimental
.........................................................................173
19.3.1
Preparation from P2O5
..............................................173
19.3.2
Preparation of Sugar Charcoal
.................................174
19.3.3
Preparation from Ca3(PO4)2
.....................................174
19.3.4
Determination of PC13
..............................................176
References
........................................................................................177
Chapter
20
Sulfur Trioxide and Oleum
..............................................................179
Summary
..........................................................................................179
Applications
.....................................................................................179
20.1
Introduction
...........................................................................179
20.2
Discussion
..............................................................................181
20.2.1
The
ЅОз-НјО
System
..............................................181
20.2.2
The SOj-HjO-Na^C^ System
................................182
20.3
Experimental
.........................................................................182
References
........................................................................................185
Chapter
21
Thionyl Chloride and Chlorosulfonic Acid
......................................187
Summary
..........................................................................................187
Applications
.....................................................................................187
21.1
Introduction
...........................................................................187
21.2
Discussion
..............................................................................189
21.2.1
The S/Clj System
......................................................190
21.2.2
Purification of SOC12
................................................191
21.2.3
Separation of HSOjCl and S2O5C12
..........................191
21.3
Experimental
.........................................................................192
21.3.1
Preparation of Sulfur Monochloride S2C12
...............192
21.3.2
Preparation of Sulfur Dichloride SC12
.....................192
21.3.3
Preparation of SOC12 and HSOjCl
...........................194
21.3.4
Purification of SOC12
................................................195
References
........................................................................................196
Appendix: Assay of Reagents
..............................................................................199
Index
......................................................................................................................213
|
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| id | DE-604.BV037383072 |
| illustrated | Illustrated |
| indexdate | 2024-07-09T23:23:07Z |
| institution | BVB |
| isbn | 9781439813126 |
| language | English |
| lccn | 2010038460 |
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| owner_facet | DE-11 DE-703 |
| physical | XV, 217 S. Ill., graph. Darst. |
| publishDate | 2011 |
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| publishDateSort | 2011 |
| publisher | CRC Press |
| record_format | marc |
| spelling | Lerner, Leonid Verfasser aut Small-scale synthesis of laboratory reagents with reaction modeling Leonid Lerner Boca Raton [u.a.] CRC Press 2011 XV, 217 S. Ill., graph. Darst. txt rdacontent n rdamedia nc rdacarrier Includes bibliographical references and index Chemie Chemical tests and reagents Synthesis SCIENCE / Chemistry / Industrial & Technical bisacsh Chemische Synthese (DE-588)4133806-6 gnd rswk-swf Anorganische Verbindungen (DE-588)4002147-6 gnd rswk-swf Anorganische Verbindungen (DE-588)4002147-6 s Chemische Synthese (DE-588)4133806-6 s DE-604 Digitalisierung UB Bayreuth application/pdf http://bvbr.bib-bvb.de:8991/F?func=service&doc_library=BVB01&local_base=BVB01&doc_number=022536156&sequence=000002&line_number=0001&func_code=DB_RECORDS&service_type=MEDIA Inhaltsverzeichnis |
| spellingShingle | Lerner, Leonid Small-scale synthesis of laboratory reagents with reaction modeling Chemie Chemical tests and reagents Synthesis SCIENCE / Chemistry / Industrial & Technical bisacsh Chemische Synthese (DE-588)4133806-6 gnd Anorganische Verbindungen (DE-588)4002147-6 gnd |
| subject_GND | (DE-588)4133806-6 (DE-588)4002147-6 |
| title | Small-scale synthesis of laboratory reagents with reaction modeling |
| title_auth | Small-scale synthesis of laboratory reagents with reaction modeling |
| title_exact_search | Small-scale synthesis of laboratory reagents with reaction modeling |
| title_full | Small-scale synthesis of laboratory reagents with reaction modeling Leonid Lerner |
| title_fullStr | Small-scale synthesis of laboratory reagents with reaction modeling Leonid Lerner |
| title_full_unstemmed | Small-scale synthesis of laboratory reagents with reaction modeling Leonid Lerner |
| title_short | Small-scale synthesis of laboratory reagents |
| title_sort | small scale synthesis of laboratory reagents with reaction modeling |
| title_sub | with reaction modeling |
| topic | Chemie Chemical tests and reagents Synthesis SCIENCE / Chemistry / Industrial & Technical bisacsh Chemische Synthese (DE-588)4133806-6 gnd Anorganische Verbindungen (DE-588)4002147-6 gnd |
| topic_facet | Chemie Chemical tests and reagents Synthesis SCIENCE / Chemistry / Industrial & Technical Chemische Synthese Anorganische Verbindungen |
| url | http://bvbr.bib-bvb.de:8991/F?func=service&doc_library=BVB01&local_base=BVB01&doc_number=022536156&sequence=000002&line_number=0001&func_code=DB_RECORDS&service_type=MEDIA |
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