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

HRID 889792노트

반응식

HRID 889792 반응식
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]

참가 물질

4

반응물 2

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

생성물 1

HCID 5128448Lithium bis(dimethylethylsilyl)amide

시약·촉매·용매 1

HCID 8058Hexane용매2회

실험 절차

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:

후처리

  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.

출처 및 근거

ORD 기록
ord-1e36c61fa6114ead93486d0ec4e78ad6
출처 데이터셋
uspto-grants-2006_02
특허 번호
US06994800B1

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