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Pyridine → [2-(Diethoxymethyl)phenyl](2-fluorophenyl)-methanone

HRID 1422128
ノート
印刷プレビュー

反応式

HRID 1422128 の反応式
N1C=CC=CC=1.O=[Si]=O.[CH2:10]([O:12][CH:13]([O:29][CH2:30][CH3:31])[C:14]1[CH:19]=[CH:18][CH:17]=[CH:16][C:15]=1[CH:20]([C:22]1[CH:27]=[CH:26][CH:25]=[CH:24][C:23]=1[F:28])[OH:21])[CH3:11]>[O-2].[O-2].[O-2].[Cr+6].ClCCl>[CH2:30]([O:29][CH:13]([O:12][CH2:10][CH3:11])[C:14]1[CH:19]=[CH:18][CH:17]=[CH:16][C:15]=1[C:20]([C:22]1[CH:27]=[CH:26][CH:25]=[CH:24][C:23]=1[F:28])=[O:21])[CH3:31]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

HCID 1049PyridineHCID 24261SilicaHCID 183575462-(Diethoxymethyl)-alpha-(2-fluorophenyl)-benzenemethanol

生成物 1

HCID 18357461[2-(Diethoxymethyl)phenyl](2-fluorophenyl)-methanone収率 94.7%

試薬・触媒・溶媒 2

HCID 6344Dichloromethane溶媒2 回
HCID 10219390
chromium (VI) trioxide
溶媒

実験手順

Under a nitrogen atmosphere, 758 ml of pyridine and 469 g of dicalite were added to 6 l of dry dichloromethane. In one portion 469 g of chromium trioxide were added under vigorous stirring. The resulting mixture was stirred at room temperature for 0.5 h, after which a solution of 238 g of 2-(diethoxymethyl)-α-(2-fluorophenyl)-benzenemethanol in 600 ml dry dichloromethane was added. After stirring at room temperature for 2 h, the mixture was filtered. The filtrate was washed with 3×1 l of 1N sodium hydroxide in water and 1 l of water, dried over magnesium sulphate and evaporated to dryness under reduced pressure to yield 224 g of [2-(diethoxymethyl)phenyl](2-fluorophenyl)-methanone as an oil, M.S. (C.I.) (M/Z): 303 [M+H]+.

後処理

  1. stirringAfter stirring at room temperature for 2 h
  2. filtrationthe mixture was filtered
  3. washThe filtrate was washed with 3×1 l of 1N sodium hydroxide in water and 1 l of water
  4. dry with materialdried over magnesium sulphate
  5. customevaporated to dryness under reduced pressure

出典と根拠

ORDレコード
ord-4047409c32914fd89f5d465eaf16a581
出典データセット
uspto-grants-2000_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06080773

反応ノート

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