2-(Chloromethyl)-3,4-dimethoxypyridin-1-ium chloride → HCID 178493203、化合物

HRID 845518ノート

反応式

HRID 845518 の反応式
[Cl-].Cl[CH2:3][C:4]1[C:9]([O:10][CH3:11])=[C:8]([O:12][CH3:13])[CH:7]=[CH:6][NH+:5]=1.[SH:14][C:15]1[NH:19][C:18]2[CH:20]=[CH:21][C:22]([O:24][C:25]([F:30])([F:29])[CH:26]([F:28])[F:27])=[CH:23][C:17]=2[N:16]=1>C(O)C.O.[OH-].[Na+]>[CH3:11][O:10][C:9]1[C:4]([CH2:3][S:14][C:15]2[NH:19][C:18]3[CH:20]=[CH:21][C:22]([O:24][C:25]([F:30])([F:29])[CH:26]([F:28])[F:27])=[CH:23][C:17]=3[N:16]=2)=[N:5][CH:6]=[CH:7][C:8]=1[O:12][CH3:13]

参加物

6

反応物 2

HCID 248204092-(Chloromethyl)-3,4-dimethoxypyridin-1-ium chlorideHCID 178506049HCID 178506049、化合物

生成物 1

HCID 178493203HCID 178493203、化合物

試薬・触媒・溶媒 3

HCID 702Ethanol溶媒HCID 962Water溶媒2 回HCID 14798Sodium Hydroxide溶媒

反応条件

温度
20 °C

実験手順

0.38 g (1.7 mmol) of 2-chloromethyl-3,4-dimethoxypyridinium chloride is added to a solution of 0.46 g (1.7 mmol) of 2-mercapto-5-(1,1,2,2-tetra fluoroethoxy)-1H-benzimidazole in 10 ml of ethanol, 10 ml of water and 1.8 ml of 2N sodium hydroxide solution; after the mixture has been stirred at 20° C. for one hour, a further 10 ml of water are added dropwise. The mixture is then stirred at 20° C. for a further four hours. The solid which has precipitated out is filtered off, washed with 0.01N sodium hydroxide solution and then with water until neutral and dried to constant weight. 0.63 g (90% of theory) of the title compound is obtained as a colorless crystalline powder of m.p. 98°-102° C.

後処理

  1. stirringThe mixture is then stirred at 20° C. for a further four hours
  2. customThe solid which has precipitated out
  3. filtrationis filtered off
  4. washwashed with 0.01N sodium hydroxide solution
  5. dry with materialwith water until neutral and dried to constant weight

出典と根拠

ORDレコード
ord-b61163aa447a43309b6dc8594a674096
出典データセット
uspto-grants-1988_07
特許番号
US04758579

反応ノート

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