HRID898798

反应详情

EQUATION

反应方程式

HRID 898798 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

4-[2-(9-Oxa-3,7-diazabicyclo[3.3.1]non-3-yl)ethoxy]benzonitrile (0.80 g, 2.92 mmol, see preparation D above) was dissolved in MeCN (30 mL) and mixed with 4-(4-chlorobutyl)pyridine (0.74 g, 4.39 mmol, from step (i) above) and K2CO3 (1.62 g, 11.71 mmol). 1 drop of Br2 was added and the mixture was refluxed for 24 h. The mixture was filtered and evaporated. Purification by chromatography on silica, eluting with DCM:4% MeOH (satd. with ammonia), gave 0.68 g (57.2%) of the title compound.

WORKUP

后处理

  1. temperaturethe mixture was refluxed for 24 h
  2. filtrationThe mixture was filtered
  3. customevaporated
  4. customPurification by chromatography on silica
  5. washeluting with DCM