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

HRID 370782
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HRID 370782 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[CH:39]=[CH:38][CH:37]=[CH:36][C:35]=3[F:40])[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][CH:37]=[CH:36][C:35]=3[F:40])=[O:9])[NH:23][C:24]=2[C:25]2[CH:30]=[CH:29][C:28]([O:31][CH3:32])=[CH:27][CH:26]=2)=[CH:18][CH:19]=1
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참가 물질

4

반응물 2

HCID 70297m-Chloroperbenzoic acidHCID 128323074,5-Bis(4-methoxyphenyl)-2-(2-fluorophenylthio)imidazole

생성물 1

HCID 128323414,5-Bis(4-methoxyphenyl)-2-(2-fluorophenylsulfinyl)imidazole수율 82.5%

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 4.07 g of 4,5-bis(4-methoxyphenyl)-2-(2-fluorophenylthio)imidazole in 100 ml of dichloromethane. The solution is stirred for 3 hours at room temperature, 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 obtaining 3.49 g of 4,5-bis(4-methoxyphenyl)-2-(2-fluorophenylsulfinyl)imidazole as an amorphous foam.

후처리

  1. washwashed 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

출처 및 근거

ORD 기록
ord-954b1f0d220542de8797227a3591c1e7
출처 데이터셋
uspto-grants-1985_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04528298

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