Water → HCID 54493231、化合物

HRID 980831ノート

反応式

HRID 980831 の反応式
[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]

参加物

6

反応物 3

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

生成物 1

HCID 54493231HCID 54493231、化合物収率 30%

試薬・触媒・溶媒 2

HCID 8082Piperidine触媒HCID 1140Toluene溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-4d2caf933022410fbca0a5412cca2120
出典データセット
uspto-grants-1987_01
特許番号
US04639447

反応ノート

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