Tetramethoxysilane → HCID 178503003、化合物

HRID 48096

反応式

HRID 48096 の反応式
[Mg].[F:2][C:3]([F:27])([F:26])[O:4][C:5]1[CH:10]=[CH:9][C:8]([C@H:11]2[CH2:16][CH2:15][C@H:14]([C@H:17]3[CH2:22][CH2:21][C@H:20]([CH2:23][CH2:24]Cl)[CH2:19][CH2:18]3)[CH2:13][CH2:12]2)=[CH:7][CH:6]=1.[CH3:28][O:29][Si:30](OC)([O:33][CH3:34])[O:31][CH3:32]>C1COCC1>[F:2][C:3]([F:27])([F:26])[O:4][C:5]1[CH:10]=[CH:9][C:8]([C@H:11]2[CH2:16][CH2:15][C@H:14]([C@H:17]3[CH2:22][CH2:21][C@H:20]([CH2:23][CH2:24][Si:30]([O:33][CH3:34])([O:31][CH3:32])[O:29][CH3:28])[CH2:19][CH2:18]3)[CH2:13][CH2:12]2)=[CH:7][CH:6]=1

参加物

5

反応物 3

HCID 12682TetramethoxysilaneHCID 5462224MagnesiumHCID 178506380HCID 178506380、化合物

生成物 1

HCID 178503003HCID 178503003、化合物収率 57%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

実験手順

A Grignard reagent was prepared from 100 ml of THF, magnesium (120 mmole) and 1-trifluoromethoxy-4-(trans-4-(trans-4-chloroethylcyclohexyl)cyclohexyl)benzene (100 mmole) under nitrogen atmosphere. A THF 100 ml solution of tetramethoxysilane (150 mmole) was heated to 65° C., and the Grignard reagent was added dropwise thereto. The solution was stirred at the same temperature for 2 hours, and after left standing for cooling, the reaction mixture was filtered. The solvent was distilled off, and then 1-trifluoromethoxy-4-(trans-4-(trans-4-trimethoxysilylethylcyclohexyl)cyclohexyl)benzene (57 mmole) was obtained by distillation under reduced pressure.

後処理

  1. waitafter left standing
  2. temperaturefor cooling
  3. filtrationthe reaction mixture was filtered
  4. distillationThe solvent was distilled off

出典と根拠

ORDレコード
ord-c5317193ef2e4833bc7f47c236f2fa9b
出典データセット
uspto-grants-2004_03
特許番号
US06703083B2

関連ノート

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