HRID1761862

反应详情

EQUATION

反应方程式

HRID 1761862 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

13 ml of 28% methanolic solution of sodium methoxide were added to a solution of 5.0 g of 4-mercaptoquinazoline and 5.5 g of 2-chloromethyl-4-methylpyridine hydrochloride in 50 ml of methanol and stirred at room temperature for 5 hours. A reaction solution was poured into water and extracted with chloroform. The chloroform layer was washed with an aqueous sodium carbonate solution, dried over sodium sulfate and distilled off under reduced pressure. The residue was purified by silica gel column chromatography. The fraction eluted with 10% ethyl acetate/chloroform was crystallized from isopropyl ether to obtain 1.84 g (22.3%) of the title compound.

WORKUP

后处理

  1. extractionextracted with chloroform
  2. washThe chloroform layer was washed with an aqueous sodium carbonate solution
  3. dry with materialdried over sodium sulfate
  4. distillationdistilled off under reduced pressure
  5. customThe residue was purified by silica gel column chromatography
  6. washThe fraction eluted with 10% ethyl acetate/chloroform
  7. customwas crystallized from isopropyl ether