Ammonia → HCID 178488165、化合物

HRID 867891

反応式

HRID 867891 の反応式
ClC1C=CC=C(C(OO)=[O:9])C=1.[CH3:12][O:13][C:14]1[CH:37]=[CH:36][C:17]2[NH:18][C:19]([S:21][CH2:22][C:23]3[C:28]([CH3:29])=[C:27]([N:30]4[CH2:35][CH2:34][CH2:33][CH2:32][CH2:31]4)[N:26]=[CH:25][N:24]=3)=[N:20][C:16]=2[CH:15]=1.N>ClCCl>[CH3:12][O:13][C:14]1[CH:37]=[CH:36][C:17]2[NH:18][C:19]([S:21]([CH2:22][C:23]3[C:28]([CH3:29])=[C:27]([N:30]4[CH2:35][CH2:34][CH2:33][CH2:32][CH2:31]4)[N:26]=[CH:25][N:24]=3)=[O:9])=[N:20][C:16]=2[CH:15]=1

参加物

5

反応物 3

HCID 222AmmoniaHCID 70297m-Chloroperbenzoic acidHCID 178488135HCID 178488135、化合物

生成物 1

HCID 178488165HCID 178488165、化合物

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

A solution of m-chloroperbenzoic acid (2.16 g) in dichloromethane (40 ml) was added to a stirred solution of 5-methoxy-2-(5-methyl-6-piperidino-4-pyrimidinylmethylthio)-(1H)-benzimidazole (4.0 g) in dichloromethane (110 ml) cooled to between -40° and -50°. After a further hour at -40°, ammonia was passed through the reaction mixture and the precipitated solid filtered off. The filtrate was stripped, and the residual glass triturated with acetonitrile to give 5-methoxy-2-(5-methyl-6-piperidino-4-pyrimidinylmethylsulphinyl)-(1H)-benzimidazole, 2.66 g, m.p. 87°-89°.

後処理

  1. temperaturecooled to between -40° and -50°
  2. waitAfter a further hour at -40°
  3. filtrationthe precipitated solid filtered off
  4. customthe residual glass triturated with acetonitrile

出典と根拠

ORDレコード
ord-0c90fdba4eb9430090452e771d6b5fee
出典データセット
uspto-grants-1988_10
特許番号
US04777172

関連ノート

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