HRID1995297

反应详情

EQUATION

反应方程式

HRID 1995297 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 1,2,3,4-tetrahydro-8,9-dimethyl-5H-[1]benzopyrano[3,4-c]pyridin-5-one (6.0 g, 0.026 moles), triethylamine (6.1 g, 0.060 moles), and 3-(2-chloroethyl)-3-azabicyclo[3.2.2]nonane hydrochloride (6.3 g, 0.028 moles) in absolute ethanol (150 ml) is stirred at reflux under a nitrogen atmosphere for 24 hours. The crude product precipitates as the free base as the reaction mixture is cooled slowly to room temperature. The product is filtered and recrystallized from absolute ethanol to yield the final product (4.6 g), mp 174°-175° C.

WORKUP

后处理

  1. temperatureat reflux under a nitrogen atmosphere for 24 hours
  2. customThe crude product precipitates as the free base as the reaction mixture
  3. filtrationThe product is filtered
  4. customrecrystallized from absolute ethanol