HRID597248

反应详情

EQUATION

反应方程式

HRID 597248 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 10 g (0.043 m) of 1,2,3,4-tetrahydro-8-methoxy-5H-[1]benzopyrano [3,4-c]pyridin-5-one, 11.2 g (0.06 m) of N-(2-chloroethyl)-morpholine HCl and 14.2 g of triethylamine (0.14 m) in 170 ml of abs. EtOH was refluxed with stirring and protection from moisture for 4 hours. The reaction was filtered hot, cooled slightly and treated with dry HCl. The resulting precipitate was filtered and washed with EtOH, then ether; yield 14.6 g (81%). Crystallization from methanol afforded analytical material, mp 237°-40° C.

WORKUP

后处理

  1. filtrationThe reaction was filtered hot
  2. temperaturecooled slightly
  3. additiontreated with dry HCl
  4. filtrationThe resulting precipitate was filtered
  5. washwashed with EtOH
  6. customCrystallization from methanol afforded analytical material, mp 237°-40° C.