4-Chlorobutyrophenone → 2-(4-Chloro-1-phenyl-butylidene)-N-phenyl-hydrazinecarbothioamide

HRID 613683

反応式

HRID 613683 の反応式
[Cl:1][CH2:2][CH2:3][CH2:4][C:5]([C:7]1[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=1)=O.[C:13]1([NH:19][C:20](=[S:23])[NH:21][NH2:22])[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=1>C(O)C>[Cl:1][CH2:2][CH2:3][CH2:4][C:5](=[N:22][NH:21][C:20](=[S:23])[NH:19][C:13]1[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=1)[C:7]1[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=1

参加物

4

反応物 2

HCID 2535334-ChlorobutyrophenoneHCID 730679Hydrazinecarbothioamide, N-phenyl-

生成物 1

HCID 537472602-(4-Chloro-1-phenyl-butylidene)-N-phenyl-hydrazinecarbothioamide収率 62.6%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

A mixture of 4-chlorobutyrophenone (6.7 mL, 42 mmol) and 4-phenyl-3-thiosemicarbazide (7.0 g, 42 mmol) in 500 mL of ethanol was warmed under a nitrogen atmosphere to dissolve all the solids and then the reaction stirred at room temperature for four days. The solid formed was collected by filtration and dried under reduced pressure to give 8.73 g of a white solid. Recrystallization of the solid from ethanol gave 7.99 g (57%) of the title compound as a white solid, mp 107-109° C.

後処理

  1. temperaturewas warmed under a nitrogen atmosphere
  2. dissolutionto dissolve all the solids
  3. customThe solid formed
  4. filtrationwas collected by filtration
  5. customdried under reduced pressure

出典と根拠

ORDレコード
ord-a4ace6d1b5ed443c8dd624f2fd2543b9
出典データセット
uspto-grants-1999_12
特許番号
US06008362

関連ノート

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