1,3-Diethyl-1,1,3,3-tetramethyldisilazane → Lithium bis(dimethylethylsilyl)amide

HRID 889792ノート

反応式

HRID 889792 の反応式
C([Li:5])CCC.[CH2:6]([Si:8]([NH:11][Si:12]([CH3:16])([CH3:15])[CH2:13][CH3:14])([CH3:10])[CH3:9])[CH3:7]>CCCCCC>[CH2:13]([Si:12]([N-:11][Si:8]([CH3:9])([CH3:10])[CH2:6][CH3:7])([CH3:15])[CH3:16])[CH3:14].[Li+:5]

参加物

4

反応物 2

HCID 1403021,3-Diethyl-1,1,3,3-tetramethyldisilazaneHCID 178418339Butyllithium

生成物 1

HCID 5128448Lithium bis(dimethylethylsilyl)amide

試薬・触媒・溶媒 1

HCID 8058Hexane溶媒2 回

実験手順

Lithium bis(ethyldimethylsilyl)amide was prepared by the slow addition via syringe of a hexane solution of butyl lithium (50.6 mL of 2.73 M solution, 138 mmol) to a stirred hexane solution (100 mL) of bis(ethyldimethylsilyl)amine (26.2 g, 138 mmol) at room temperature. Stirring was continued for one hour and the solution was then refluxed for one hour. The hexane was evaporated under vacuum, leaving a pale yellow liquid. It was distilled at a temperature of 123° C. and a pressure of 0.2 torr to yield 23.2 g (86%) of clear liquid lithium bis(ethyldimethylsilyl)amide. Its viscosity was measured to be 37.5 centipoise at 40° C. Its NMR parameters are as follows:

後処理

  1. temperaturethe solution was then refluxed for one hour
  2. customThe hexane was evaporated under vacuum
  3. customleaving a pale yellow liquid
  4. distillationIt was distilled at a temperature of 123° C.

出典と根拠

ORDレコード
ord-1e36c61fa6114ead93486d0ec4e78ad6
出典データセット
uspto-grants-2006_02
特許番号
US06994800B1

反応ノート

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