反应详情

温度

4 °C

A solution of 2-[(3-chloro-2-chloromethyl-pyridin-4-yl)-methyl-amino]-ethanol isolated in step a) (10.2 g) and 2-mercapto-benzimidazole (5.8 g, 39 mmol) in 2-propanol (250 ml) is boiled under reflux for 2 h. After cooling to 4° C. the precipitate is filtered, washed with 2-propanol and dried in vacuo. The residue is dissolved in water, adjusted to pH 8 with aqueous sodium bicarbonate solution and extracted with ethyl acetate. The combined organic extracts are washed with water, dried over magnesium sulfate and evaporated in vacuo. The residue is crystallized from ethyl acetate to give the title compound as an off-white solid, 7.9 g (58%). M.p. 132-5° C.

1. temperatureunder reflux for 2 h
2. filtrationis filtered
3. washwashed with 2-propanol
4. customdried in vacuo
5. dissolutionThe residue is dissolved in water
6. extractionextracted with ethyl acetate
7. washThe combined organic extracts are washed with water
8. dry with materialdried over magnesium sulfate
9. customevaporated in vacuo
10. customThe residue is crystallized from ethyl acetate