Gallium, chlorodimethyl- → o-Trifluoromethylbenzyldimethylgallium

HRID 2372542ノート

反応式

HRID 2372542 の反応式
[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]

参加物

6

反応物 3

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

生成物 1

HCID 14692906o-Trifluoromethylbenzyldimethylgallium

試薬・触媒・溶媒 2

HCID 8058Hexane溶媒HCID 21584099Diethylether hexane溶媒2 回

実験手順

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°.

後処理

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

出典と根拠

ORDレコード
ord-7db2b241997c47a39394763b74c9d79f
出典データセット
uspto-grants-1992_03
特許番号
US05099044

反応ノート

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