m-Chloroperbenzoic acid → 4,5-Bis(4-methoxyphenyl)-2-(2,4-difluorophenylsulfinyl)imidazole

HRID 1995216ノート

反応式

HRID 1995216 の反応式
ClC1C=CC=C(C(OO)=[O:9])C=1.[CH3:12][O:13][C:14]1[CH:19]=[CH:18][C:17]([C:20]2[N:21]=[C:22]([S:33][C:34]3[CH:39]=[CH:38][C:37]([F:40])=[CH:36][C:35]=3[F:41])[NH:23][C:24]=2[C:25]2[CH:30]=[CH:29][C:28]([O:31][CH3:32])=[CH:27][CH:26]=2)=[CH:16][CH:15]=1>ClCCl>[CH3:12][O:13][C:14]1[CH:15]=[CH:16][C:17]([C:20]2[N:21]=[C:22]([S:33]([C:34]3[CH:39]=[CH:38][C:37]([F:40])=[CH:36][C:35]=3[F:41])=[O:9])[NH:23][C:24]=2[C:25]2[CH:26]=[CH:27][C:28]([O:31][CH3:32])=[CH:29][CH:30]=2)=[CH:18][CH:19]=1

参加物

4

反応物 2

HCID 70297m-Chloroperbenzoic acidHCID 128323094,5-Bis(4-methoxyphenyl)-2-(2,4-difluorophenylthio)imidazole

生成物 1

HCID 128323494,5-Bis(4-methoxyphenyl)-2-(2,4-difluorophenylsulfinyl)imidazole収率 73.9%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

A solution of 2.164 g of 3-chloroperbenzoic acid (80%) in 150 ml of dichloromethane is added dropwise to a solution of 4.25 g of 4,5-bis(4-methoxyphenyl)-2-(2,4-difluorophenylthio)imidazole in 100 ml of dichloromethane. The mixture is agitated for 3 hours at room temperature, the solution washed with sodium bicarbonate solution, dried over sodium sulfate, and concentrated under vacuum to dryness. The residue is chromatographed on 150 g of silica gel with acetone/hexane, thus producing 3.26 g of 4,5-bis(4-methoxyphenyl)-2-(2,4-difluorophenylsulfinyl)imidazole as an amorphous foam.

後処理

  1. washthe solution washed with sodium bicarbonate solution
  2. dry with materialdried over sodium sulfate
  3. concentrationconcentrated under vacuum to dryness
  4. customThe residue is chromatographed on 150 g of silica gel with acetone/hexane

出典と根拠

ORDレコード
ord-683dc1c61a284309a14ef80559484f4d
出典データセット
uspto-grants-1983_09
特許番号
US04402960

反応ノート

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