HRID1655230

反应详情

EQUATION

反应方程式

HRID 1655230 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

5N NaOH (3.39 ml) was added dropwise to a stirred solution of 2-chloromethyl-3-fluoro-4-morpholinopyridine hydrochloride (2.06 g) and 5-methoxy-(1H)-benzimidazole-2-thiol (1.39 g) in ethanol (35 ml). After 3 hours excess solvent was removed and the residue treated with water (80 ml) and extracted with dichloromethane. The extracts were washed with water, dried (K2CO3), excess solvent removed and the residue crystallised from ethyl acetate to yield 2-(4-morpholino-3-fluoro-2-pyridylmethylthio)-5-methoxy-(1H)-benzimidazole (2.16 g) m.p. 121°-123°.

WORKUP

后处理

  1. customAfter 3 hours excess solvent was removed
  2. additionthe residue treated with water (80 ml)
  3. extractionextracted with dichloromethane
  4. washThe extracts were washed with water
  5. dry with materialdried (K2CO3), excess solvent
  6. customremoved
  7. customthe residue crystallised from ethyl acetate