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

HRID 370795노트

반응식

HRID 370795 반응식
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[N:39]=[CH:38][CH:37]=[CH:36][N:35]=3)[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>[CH3:32][O:31][C:28]1[CH:27]=[CH:26][C:25]([C:24]2[N:23]=[C:22]([S:33]([C:34]3[N:39]=[CH:38][CH:37]=[CH:36][N:35]=3)=[O:9])[NH:21][C:20]=2[C:17]2[CH:18]=[CH:19][C:14]([O:13][CH3:12])=[CH:15][CH:16]=2)=[CH:30][CH:29]=1

참가 물질

4

반응물 2

HCID 70297m-Chloroperbenzoic acidHCID 128322954,5-Bis(4-methoxyphenyl)-2-(2-pyrimidylthio)imidazole

생성물 1

HCID 128323674,5-Bis(4-methoxyphenyl)-2-(2-pyrimidinylsulfinyl)imidazole수율 86.5%

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

A solution of 2.164 g of 3-chloroperbenzoic acid (80%) in 150 ml of dichloromethane is added dropwise to a solution of 3.91 g of 4,5-bis(4-methoxyphenyl)-2-(2-pyrimidinylthio)imidazole in 100 ml of dichloromethane. The mixture is stirred for 3 hours at room temperature, the solution is washed with sodium bicarbonate solution, dried over sodium sulfate, and concentrated to dryness under vacuum. The residue is chromatographed on 150 g of silica gel with acetone/hexane, thus producing 3.52 g of 4,5-bis(4-methoxyphenyl)-2-(2-pyrimidinylsulfinyl)imidazole as an amorphous foam.

후처리

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

출처 및 근거

ORD 기록
ord-74532e9eafbc46d59d6e620bafbf45ee
출처 데이터셋
uspto-grants-1985_07
특허 번호
US04528298

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