HRID1992356

反应详情

EQUATION

反应方程式

HRID 1992356 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
60 °C

PROCEDURE

实验过程

A suspension of 4-[2-(9-Oxa-3,7-diaza-bicyclo[3.3.1]non-3-yl)-ethoxy]-benzonitrile (6.5 g, 0.02 mol, see WO 01/28992), (3-Bromo-propyl)-carbamic acid tert-butyl ester (6.0 g, 0.025 mol) and dry K2CO3 (13.08 g, 0.0946 mol) in 40 ml of dry acetonitrile was stirred at 60° C. overnight under N2 atmosphere. The reaction mixture was filtered through celite and the filtrate was concentrated under reduced pressure. The residue was purified by column chromatography over silica gel using 20% ethyl acetate in petroleum ether as eluent to yield sub-title compound (3.5 g) as a liquid.

WORKUP

后处理

  1. filtrationThe reaction mixture was filtered through celite
  2. concentrationthe filtrate was concentrated under reduced pressure
  3. customThe residue was purified by column chromatography over silica gel using 20% ethyl acetate in petroleum ether as eluent