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Water → 2-Amino-4-ethylthio-1-(3-methoxycarbonyl-2-thioureido)benzene

HRID 258761
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HRID 258761 반응식
[CH2:1]([S:3][C:4]1[CH:9]=[CH:8][C:7]([NH:10][C:11]([NH:13][C:14]([O:16][CH3:17])=[O:15])=[S:12])=[C:6]([N+:18]([O-])=O)[CH:5]=1)[CH3:2].O>CO>[NH2:18][C:6]1[CH:5]=[C:4]([S:3][CH2:1][CH3:2])[CH:9]=[CH:8][C:7]=1[NH:10][C:11]([NH:13][C:14]([O:16][CH3:17])=[O:15])=[S:12]
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참가 물질

4

반응물 2

HCID 962WaterHCID 203720534-Ethylthio-1-(3-methoxycarbonyl-2-thioureido)-2-nitrobenzene

생성물 1

HCID 203720472-Amino-4-ethylthio-1-(3-methoxycarbonyl-2-thioureido)benzene수율 59.2%

시약·촉매·용매 1

HCID 887Methanol용매2회

실험 절차

A mixture of 4-ethylthio-1-(3-methoxycarbonyl-2-thioureido)-2-nitrobenzene (14.0 g.), ferrous chloride tetrahydrate (3.04 g.), methanol (235 ml.) and water (50 ml.) was heated to reflux and treated with reduced iron powder (15.5 g.) portionwise during 5 minutes. The mixture was heated at reflux with stirring for one hour. Methanol (250 ml.) was added and the mixture was again heated to reflux. The hot mixture was filtered and the filtrate was allowed to cool to room temperature. The solid which crystallised on cooling was filtered off to give 2-amino-4-ethylthio-1-(3-methoxycarbonyl-2-thioureido)benzene (7.5 g.), m.p. 168° C.

후처리

  1. temperaturewas heated
  2. temperatureto reflux
  3. temperatureThe mixture was heated
  4. temperatureat reflux
  5. temperaturethe mixture was again heated to reflux
  6. filtrationThe hot mixture was filtered
  7. customThe solid which crystallised
  8. temperatureon cooling
  9. filtrationwas filtered off

출처 및 근거

ORD 기록
ord-7c8ad2b44c48474cb5eb69917516bdcf
출처 데이터셋
uspto-grants-1977_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04034107

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