Pyridine → HCID 20030580、化合物

HRID 232016

反応式

HRID 232016 の反応式
C(Cl)(=O)C([Cl:4])=O.[C:7]([C:9]1[N:17]=[CH:16][CH:15]=[CH:14][C:10]=1[C:11]([O-:13])=[O:12])#[N:8].[K+].[CH:19](Cl)(O)[CH:20]([Cl:22])[Cl:21].N1C=CC=CC=1>ClCCl.O>[C:7]([C:9]1[N:17]=[CH:16][CH:15]=[CH:14][C:10]=1[C:11]([O:13][CH2:19][C:20]([Cl:22])([Cl:4])[Cl:21])=[O:12])#[N:8]

参加物

7

反応物 4

HCID 1049PyridineHCID 65578Oxalyl chlorideHCID 1194271,1,2-TrichloroethanolHCID 23690323HCID 23690323、化合物

生成物 1

HCID 20030580HCID 20030580、化合物収率 78%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6344Dichloromethane溶媒2 回

実験手順

Oxalyl chloride (2.8 g; 0.022 mol) is added to a suspension of compound 3 (4.1 g; 0.022 mol) in dichloromethane (50 cc). The mixture is heated under reflux until gas evolution ceases and then treated with a solution of trichloroethanol (3.3 g; 0.022 mol) and pyridine (3.5 g; 0.044 mol) in dichloromethane (30 cc). The mixture is then treated with water and then dried. After evaporation of the solvent and crystallization in pentane, 2,2,2-tri-chloroethyl 2-cyanonicotinate (4.55 g; m.p. 103° C.) is obtained (yield=78%).

後処理

  1. temperatureThe mixture is heated
  2. temperatureunder reflux until gas evolution ceases
  3. customdried
  4. customAfter evaporation of the solvent and crystallization in pentane

出典と根拠

ORDレコード
ord-be80054748d5446480496c5b8647d737
出典データセット
uspto-grants-1989_07
特許番号
US04851396

関連ノート

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