Tetramethoxysilane → HCID 178503003, 화합물

HRID 48096

반응식

HRID 48096 반응식
[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

참가 물질

5

반응물 3

HCID 12682TetramethoxysilaneHCID 5462224MagnesiumHCID 178506380HCID 178506380, 화합물

생성물 1

HCID 178503003HCID 178503003, 화합물수율 57%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

실험 절차

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.

후처리

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

출처 및 근거

ORD 기록
ord-c5317193ef2e4833bc7f47c236f2fa9b
출처 데이터셋
uspto-grants-2004_03
특허 번호
US06703083B2

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