HRID1992358

反应详情

EQUATION

反应方程式

HRID 1992358 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 N-(3-Bromo-propyl)-4-cyano-benzenesulfonamide (6.39 g, 0.021 mol; see step (i) above), 9-oxa-3,7-diaza-bicyclo[3.3.1]nonane-3-carboxylic acid tert-butyl ester (4.32 g, 0.0189 mol see WO 01/28992) and dry K2CO3 (10.16 g, 0.0735 mol) in dry acetonitrile (70 ml) was stirred at 60° C. overnight under N2 atmosphere. The reaction mixture was filtered through celite and filtrate was concentrated under reduced pressure. The residue was purified by column chromatography over silica gel using 50% ethyl acetate in petroleum ether, as eluent to give the sub-title compound (4.29 g) as a solid.

WORKUP

后处理

  1. filtrationThe reaction mixture was filtered through celite and filtrate
  2. concentrationwas concentrated under reduced pressure
  3. customThe residue was purified by column chromatography over silica gel using 50% ethyl acetate in petroleum ether, as eluent