Water → HCID 54493231, 화합물

HRID 980831노트

반응식

HRID 980831 반응식
[Cl:1][C:2]1[CH:9]=[C:8]([Cl:10])[CH:7]=[CH:6][C:3]=1[CH:4]=O.[N:11]1([CH2:16][C:17]#[N:18])[CH:15]=[N:14][CH:13]=[N:12]1.O>C1(C)C=CC=CC=1.N1CCCCC1>[Cl:1][C:2]1[CH:9]=[C:8]([Cl:10])[CH:7]=[CH:6][C:3]=1[CH:4]=[C:16]([N:11]1[CH:15]=[N:14][CH:13]=[N:12]1)[C:17]#[N:18]

참가 물질

6

반응물 3

HCID 962WaterHCID 134042,4-DichlorobenzaldehydeHCID 27648382-(1H-1,2,4-triazol-1-yl)acetonitrile

생성물 1

HCID 54493231HCID 54493231, 화합물수율 30%

시약·촉매·용매 2

HCID 8082Piperidine촉매HCID 1140Toluene용매

실험 절차

138.9 g (790 millimoles) of 2,4-dichlorobenzaldehyde, 76.7 g (710 millimoles) of 2-(1,2,4-triazol-1-yl)-acetonitrile and 1 g of piperidine in 1 l of toluene are heated at the boil under a water separator until 1 equivalent of water has been separated off. The mixture is then left to cool, and the precipitated crystals are filtered off under suction. They can be purified by recrystallization from toluene. 56.5 g (30% of theory) of 3-(2,4-dichlorophenyl)-2-(1,2,4-triazol-1-yl)-acrylonitrile of melting point 156°-160° C. are obtained.

후처리

  1. customhas been separated off
  2. waitThe mixture is then left
  3. temperatureto cool
  4. filtrationthe precipitated crystals are filtered off under suction
  5. customThey can be purified by recrystallization from toluene

출처 및 근거

ORD 기록
ord-4d2caf933022410fbca0a5412cca2120
출처 데이터셋
uspto-grants-1987_01
특허 번호
US04639447

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