m-Chloroperbenzoic acid → HCID 19805451, 화합물

HRID 1681694노트

반응식

HRID 1681694 반응식
ClC1C=CC=C(C(OO)=[O:9])C=1.[CH2:12]([S:16][C:17]1[CH:22]=[CH:21][C:20]([N:23]2[C:31](=[O:32])[C:30]3[C:25](=[CH:26][CH:27]=[CH:28][CH:29]=3)[NH:24]2)=[CH:19][CH:18]=1)[CH2:13][CH2:14][CH3:15]>C(Cl)Cl>[CH2:12]([S:16]([C:17]1[CH:18]=[CH:19][C:20]([N:23]2[C:31](=[O:32])[C:30]3[C:25](=[CH:26][CH:27]=[CH:28][CH:29]=3)[NH:24]2)=[CH:21][CH:22]=1)=[O:9])[CH2:13][CH2:14][CH3:15]

참가 물질

4

반응물 2

HCID 70297m-Chloroperbenzoic acidHCID 54375321HCID 54375321, 화합물

생성물 1

HCID 19805451HCID 19805451, 화합물수율 60.7%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

3-Chloroperbenzoic acid (150mg) was added to a stirred solution of 1,2-dihydro-2-(4-butylthiophenyl)-3H-indazol-3-one (250 mg) in methylene chloride (5 ml) at 0-5° C. Stirring was continued for 15 minutes after the addition was complete. The reaction mixture was then washed with water, dried (MgSO4) and evaporated in vacuo. The residue was purified by column chromatography using methylene chloride/ether (70:30 v/v) to give 1,2-dihydro-2-(4-butylsulphinylphenyl)-3H-indazol-3-one (Ex. 52) as a solid (160 mg), m.p. 168-169° C.

후처리

  1. additionafter the addition
  2. washThe reaction mixture was then washed with water
  3. dry with materialdried (MgSO4)
  4. customevaporated in vacuo
  5. customThe residue was purified by column chromatography

출처 및 근거

ORD 기록
ord-8aa3f413e504493cacde6135f1e06f09
출처 데이터셋
uspto-grants-1992_12
특허 번호
US05173496

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