HRID2298056

反应详情

EQUATION

反应方程式

HRID 2298056 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
60 °C

PROCEDURE

实验过程

A mixture of 5-bromomethyl-2-chloro-N-(tricyclo[3.3.1.13,7]dec-1-ylmethyl)-benzamide (Example 8b, 0.130 g), 1-tertbutyloxycarbonylpiperazine (0.074 g) and diisopropylethylamine (6.3 ml) in dimethylformamide (3 ml) was heated at 60° C. for 3 h. The mixture was diluted with water (10 ml) and extracted with ethyl acetate (3×10 ml). The organic layer was dried over magnesium sulfate, filtered and the filtrate concentrated under reduced pressure. The crude material was purified on a silica gel eluting with dichloromethane/ethanol (0-20% gradient) to afford the title compound as a white foam (0.112 g).

WORKUP

后处理

  1. extractionextracted with ethyl acetate (3×10 ml)
  2. dry with materialThe organic layer was dried over magnesium sulfate
  3. filtrationfiltered
  4. concentrationthe filtrate concentrated under reduced pressure
  5. customThe crude material was purified on a silica gel eluting with dichloromethane/ethanol (0-20% gradient)