Methanethioamide → HCID 3395423, 화합물

HRID 1030456노트

반응식

HRID 1030456 반응식
[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

참가 물질

4

반응물 2

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

생성물 1

HCID 3395423HCID 3395423, 화합물수율 27.7%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

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.

후처리

  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)]

출처 및 근거

ORD 기록
ord-f69729f762b04d168eed1ce61eafa0ea
출처 데이터셋
uspto-grants-1992_04
특허 번호
US05106732

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