Methanethioamide → HCID 3395423、化合物

HRID 1030456ノート

反応式

HRID 1030456 の反応式
[CH2:1]([O:8][C:9]1[CH:14]=[CH:13][C:12]([C:15](=O)[CH2:16]Br)=[CH:11][CH:10]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[CH:19]([NH2:21])=[S:20]>C(O)C>[CH2:1]([O:8][C:9]1[CH:14]=[CH:13][C:12]([C:15]2[N:21]=[CH:19][S:20][CH:16]=2)=[CH:11][CH:10]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1

参加物

4

反応物 2

HCID 3005587MethanethioamideHCID 105425931-[4-(Benzyloxy)phenyl]-2-bromoethan-1-one

生成物 1

HCID 3395423HCID 3395423、化合物収率 27.7%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

A mixture of 4'-benzyloxy-2-bromoacetophenone (3.0 g) and thioformamide (0.63 g) in ethanol (50 ml) was refluxed under heating for 30 minutes. The reaction mixture was poured into ice-water, and the precipitating crystals were collected by filtration, extracted with diethyl ether and purified by column chromatography on silica gel [eluting solvent: methylene chloride-hexane (1:9)] to give 4-(4-benzyloxyphenyl) thiazole (720 mg, 27.7%), which was further purified by recrystallization from diethyl ether-hexane. m.p. 109°-110° C.

後処理

  1. temperaturewas refluxed
  2. temperatureunder heating for 30 minutes
  3. filtrationthe precipitating crystals were collected by filtration
  4. extractionextracted with diethyl ether
  5. custompurified by column chromatography on silica gel [eluting solvent: methylene chloride-hexane (1:9)]

出典と根拠

ORDレコード
ord-f69729f762b04d168eed1ce61eafa0ea
出典データセット
uspto-grants-1992_04
特許番号
US05106732

反応ノート

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