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4,4'-Dichlorobutyrophenone → 2-[1-(4-Chloro-phenyl)-4-chloro-butylidene]-hydrazinecarbothioamide

HRID 613686
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HRID 613686 반응식
[NH2:1][NH:2][C:3]([NH2:5])=[S:4].[Cl:6][CH2:7][CH2:8][CH2:9][C:10]([C:12]1[CH:17]=[CH:16][C:15]([Cl:18])=[CH:14][CH:13]=1)=O>CO.Cl.O>[Cl:18][C:15]1[CH:14]=[CH:13][C:12]([C:10](=[N:1][NH:2][C:3](=[S:4])[NH2:5])[CH2:9][CH2:8][CH2:7][Cl:6])=[CH:17][CH:16]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 2

HCID 27237814,4'-DichlorobutyrophenoneHCID 2723789Thiosemicarbazide

생성물 1

HCID 537421812-[1-(4-Chloro-phenyl)-4-chloro-butylidene]-hydrazinecarbothioamide수율 69.7%

시약·촉매·용매 3

HCID 313Hydrochloric Acid용매HCID 887Methanol용매HCID 962Water용매
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실험 절차

Thiosemicarbazide (9.11 g, 0.1 mol) was added under nitrogen to a solution of 4,4'-dichlorobutyrophenone (21.7 g, 0.1 mol) in 350 mL of methanol plus 27 mL of 1N HCl plus 25 mL of water and the reaction stirred at room temperature for 21 hours (overnight). The solid was collected by filtration and dried to give 20.23 g of a white solid. Recrystallization of the solid from isopropyl alcohol gave 8.37 g (29%) of the title compound as a light yellow solid, mp 125-126° C.

후처리

  1. filtrationThe solid was collected by filtration
  2. customdried

출처 및 근거

ORD 기록
ord-bfe688eb48d145caa5f48d7023f608de
출처 데이터셋
uspto-grants-1999_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06008362

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