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

HRID 613683

반응식

HRID 613683 반응식
[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

참가 물질

4

반응물 2

HCID 2535334-ChlorobutyrophenoneHCID 730679Hydrazinecarbothioamide, N-phenyl-

생성물 1

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

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-a4ace6d1b5ed443c8dd624f2fd2543b9
출처 데이터셋
uspto-grants-1999_12
특허 번호
US06008362

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