Imidazole → HCID 69987244、化合物

HRID 1634732ノート

反応式

HRID 1634732 の反応式
N1C=CN=C1.[F:6][C:7]1[CH:8]=[C:9]([C:14](=[O:16])[CH3:15])[CH:10]=[CH:11][C:12]=1[OH:13].[C:17]([Si:21]([C:29]1[CH:34]=[CH:33][CH:32]=[CH:31][CH:30]=1)([C:23]1[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=1)Cl)([CH3:20])([CH3:19])[CH3:18].O>ClCCl>[Si:21]([O:13][C:12]1[CH:11]=[CH:10][C:9]([C:14](=[O:16])[CH3:15])=[CH:8][C:7]=1[F:6])([C:17]([CH3:20])([CH3:19])[CH3:18])([C:29]1[CH:30]=[CH:31][CH:32]=[CH:33][CH:34]=1)[C:23]1[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=1

参加物

6

反応物 4

HCID 795ImidazoleHCID 962WaterHCID 94078tert-ButyldiphenylchlorosilaneHCID 27373251-(3-Fluoro-4-hydroxyphenyl)ethan-1-one

生成物 1

HCID 69987244HCID 69987244、化合物

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

To a solution of imidazole (7.29 g, 107.0 mmol) and 1-(3-fluoro-4-hydroxyphenyl)-1-ethanone (15.0 g, 97.3 mmol) in anhydrous dichloromethane (500 mL) was added drop-wise a solution of t-butyldiphenylchlorosilane (28.09 g, 102.0 mmol) in anhydrous dichloromethane (100 mL). The solution was stirred overnight at room temperature. The mixture was poured into water (500 mL) and the organic layer separated and washed with saturated sodium hydrogen carbonate, water, brine and dried over anhydrous magnesium sulfate. The solution was filtered and the solvent evaporated to dryness in vacuo to give the title compound which was used without further purification (37.9 g, 96.55 mmol). MS (APCI+, m/z): 393 [M+H]+.

後処理

  1. customthe organic layer separated
  2. washwashed with saturated sodium hydrogen carbonate, water, brine
  3. dry with materialdried over anhydrous magnesium sulfate
  4. filtrationThe solution was filtered
  5. customthe solvent evaporated to dryness in vacuo

出典と根拠

ORDレコード
ord-28c0c6158f834c21ac5ef3758b073ad8
出典データセット
uspto-grants-2003_01
特許番号
US06506901B2

反応ノート

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