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

HRID 258761
ノート
印刷プレビュー

反応式

HRID 258761 の反応式
[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]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 887Methanol溶媒2 回

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-7c8ad2b44c48474cb5eb69917516bdcf
出典データセット
uspto-grants-1977_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04034107

反応ノート

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