HRID1658745

反应详情

EQUATION

反应方程式

HRID 1658745 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

10.6 g. of 10-chloro-8-fluoro-10,11-dihydro-3-methyldibenzo[b,f]thiepin, 200 ml. of chloroform and 11.4 g. of N-methylpiperazine are heated at reflux for 30 hours. The mixture is evaporated under reduced pressure. The resulting residue is worked up via the neutral portion in essentially the same manner as described in Example 1, and there is obtained 1-{8-fluoro-10,11-dihydro-3-methyl-dibenzo[b,f]thiepin-10-yl}-4-methylpiperazine, having a melting point of 117°-121°C. By treatment with methanesulfonic acid, there is obtained the dimethanesulfonate having a melting point of 176°-178°C. (from methanol/ether).

WORKUP

后处理

  1. temperatureat reflux for 30 hours
  2. customThe mixture is evaporated under reduced pressure