Maleic Anhydride → 1-Methoxycarbonyl-3-[2-(3-carboxyacrylamido)phenyl]thiourea

HRID 1415654노트

반응식

HRID 1415654 반응식
[CH3:1][O:2][C:3]([NH:5][C:6]([NH:8][C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][C:10]=1[NH2:15])=[S:7])=[O:4].[C:16]1(=[O:22])[O:21][C:19](=[O:20])[CH:18]=[CH:17]1>C(O)C>[CH3:1][O:2][C:3]([NH:5][C:6]([NH:8][C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][C:10]=1[NH:15][C:16](=[O:22])[CH:17]=[CH:18][C:19]([OH:21])=[O:20])=[S:7])=[O:4]

참가 물질

4

반응물 2

HCID 7923Maleic AnhydrideHCID 3032830Thiophamine

생성물 1

HCID 536421621-Methoxycarbonyl-3-[2-(3-carboxyacrylamido)phenyl]thiourea수율 28.4%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

A mixture of 1-methoxycarbonyl-3-(2-aminophenyl)thiourea (10.9 g., 0.048 mole), maleic anhydride (4.7 g; 0.048 mole) and ethanol (200 ml) was boiled under reflux with stirring for one hour. The clear solution was allowed to cool and the crystals which deposited were filtered off. These were recrystallised once from ethanol and once from a mixture of acetone and petroleum spirit (b.p. 60°-80° C.) to give 1-methoxycarbonyl-3-[2-(3-carboxyacrylamido)phenyl]thiourea (4.4 g) m.p. 170°-173° C. (with decomposition).

후처리

  1. temperatureunder reflux
  2. temperatureto cool
  3. filtrationthe crystals which deposited were filtered off
  4. customThese were recrystallised once from ethanol and once from a mixture of acetone and petroleum spirit (b.p. 60°-80° C.)

출처 및 근거

ORD 기록
ord-4d05abead64c4abab4a08021772a2f2d
출처 데이터셋
uspto-grants-1977_01
특허 번호
US04005217

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