m-Chloroperbenzoic acid → HCID 19805451、化合物

HRID 1681694ノート

反応式

HRID 1681694 の反応式
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]

参加物

4

反応物 2

HCID 70297m-Chloroperbenzoic acidHCID 54375321HCID 54375321、化合物

生成物 1

HCID 19805451HCID 19805451、化合物収率 60.7%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-8aa3f413e504493cacde6135f1e06f09
出典データセット
uspto-grants-1992_12
特許番号
US05173496

反応ノート

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