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1,3-Bis(2-cyano-5-(trifluoromethyl)phenyl)triazene → 3-[4-(N,N-diethylamino)butyryl]-1,3-bis(2-cyano-5-trifluoromethylphenyl)-triazene hydrochloride

HRID 1283799
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HRID 1283799 반응식
[C:1]([C:3]1[CH:8]=[CH:7][C:6]([C:9]([F:12])([F:11])[F:10])=[CH:5][C:4]=1[N:13]=[N:14][NH:15][C:16]1[CH:21]=[C:20]([C:22]([F:25])([F:24])[F:23])[CH:19]=[CH:18][C:17]=1[C:26]#[N:27])#[N:2].[ClH:28].[CH2:29]([N:31]([CH2:38][CH3:39])[CH2:32][CH2:33][CH2:34][C:35](O)=[O:36])[CH3:30]>C(Cl)Cl>[ClH:28].[CH2:29]([N:31]([CH2:32][CH2:33][CH2:34][C:35]([N:13]([C:4]1[CH:5]=[C:6]([C:9]([F:12])([F:11])[F:10])[CH:7]=[CH:8][C:3]=1[C:1]#[N:2])[N:14]=[N:15][C:16]1[CH:21]=[C:20]([C:22]([F:23])([F:24])[F:25])[CH:19]=[CH:18][C:17]=1[C:26]#[N:27])=[O:36])[CH2:38][CH3:39])[CH3:30]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 30354951,3-Bis(2-cyano-5-(trifluoromethyl)phenyl)triazeneHCID 137955394-(Diethylamino)butanoic acid hydrochloride

생성물 1

HCID 215163883-[4-(N,N-diethylamino)butyryl]-1,3-bis(2-cyano-5-trifluoromethylphenyl)-triazene hydrochloride

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

A solution of 10.0 g. (0.026 mol.) of 1,3-bis(2-cyano-5-trifluoromethylphenyl)triazene, 6.0 g. (0.029 mol.) of N,N-dicyclohexylcarbodiimide and 5.1 g. (0.026 mol.) of 4-diethylaminobutyric acid hydrochloride in 800 ml. of methylene chloride is stirred at 25° for 12 hours. The reaction mixture is filtered and the filtrate is concentrated under reduced pressure to give a residue which is washed with ether and recrystallized from benzene to give 3-[4-(N,N-diethylamino)butyryl]-1,3-bis(2-cyano-5-trifluoromethylphenyl)-triazene hydrochloride.

후처리

  1. filtrationThe reaction mixture is filtered
  2. concentrationthe filtrate is concentrated under reduced pressure
  3. customto give a residue which
  4. washis washed with ether
  5. customrecrystallized from benzene

출처 및 근거

ORD 기록
ord-8ad6a03a424648158ac1c1c825634134
출처 데이터셋
uspto-grants-1976_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US03976633

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