Gallium, chlorodimethyl- → o-Trifluoromethylbenzyldimethylgallium

HRID 2372542노트

반응식

HRID 2372542 반응식
[F:1][C:2]([F:12])([F:11])[C:3]1[CH:10]=[CH:9][CH:8]=[CH:7][C:4]=1[CH2:5]Br.C([Li])CCC.[Cl-].[CH3:19][Ga+:20][CH3:21]>CCOCC.CCCCCC.CCCCCC>[F:1][C:2]([F:12])([F:11])[C:3]1[CH:10]=[CH:9][CH:8]=[CH:7][C:4]=1[CH2:5][Ga:20]([CH3:21])[CH3:19]

참가 물질

6

반응물 3

HCID 81329Gallium, chlorodimethyl-HCID 1230571-(Bromomethyl)-2-(trifluoromethyl)benzeneHCID 178418339Butyllithium

생성물 1

HCID 14692906o-Trifluoromethylbenzyldimethylgallium

시약·촉매·용매 2

HCID 8058Hexane용매HCID 21584099Diethylether hexane용매2회

실험 절차

5.25 g (22 mmol) of o-trifluoromethylbenzyl bromide in 10 ml of ether/hexane are added at -50° to a mixture of 45 ml of ether/hexane (2:1) and 14.7 ml (1.5N =22 mmol) of n-butyllithium. After stirring for 15 minutes, 2.1 g (16 mmol) of dimethylgallium chloride in 20 ml of hexane are added. Then the reaction mixture is allowed to come to room temperature, it is stirred for 24 hours, and the LiCl is filtered off and the solvent removed. After sublimation in vacuo, o-trifluoromethylbenzyldimethylgallium is obtained with a Mp. 35°-38°.

후처리

  1. customto come to room temperature
  2. stirringit is stirred for 24 hours
  3. filtrationthe LiCl is filtered off
  4. customthe solvent removed

출처 및 근거

ORD 기록
ord-7db2b241997c47a39394763b74c9d79f
출처 데이터셋
uspto-grants-1992_03
특허 번호
US05099044

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