HRID649218

反应详情

EQUATION

反应方程式

HRID 649218 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of 5-trifluoromethyl-2-mercaptobenzimidazole (1.10 g), 1N-sodium hydroxide (7.2 ml), and methanol (5 ml) was added a solution of 2-bromomethyl-3,4-dimethoxypyridine (1.3 g) in methanol (35 ml) at room temperature over 10 minutes. The mixture was stirred for one hour, concentrated, and extracted with chloroform. The organic layer was washed with 1N-sodium hydroxide and then with water, dried, and evaporated. The residue was purified by column chromatography on silica gel (chloroform-ethyl acetate-acetone (1:1:0.1)) and recrestallized from chloroform-isopropyl ether, to give 2-[(3,4-dimethoxypyrid-2-yl)methylthio]-5-trifluoromethylbenzimidazole (310 mg) as white crystals.

WORKUP

后处理

  1. concentrationconcentrated
  2. extractionextracted with chloroform
  3. washThe organic layer was washed with 1N-sodium hydroxide
  4. dry with materialwith water, dried
  5. customevaporated
  6. customThe residue was purified by column chromatography on silica gel (chloroform-ethyl acetate-acetone (1:1:0.1))