HRID1112447

反应详情

EQUATION

反应方程式

HRID 1112447 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

N-[[2-[3-(4-Morpholinyl)propoxy]phenyl]methyl]benzeneethanamine (14g, see Example 31C) is reacted with 9.2 g of p-chlorobenzenesulfonyl chloride in 130 ml of chloroform. A solution of the amine in chloroform is added dropwise at 10°-15° C to a stirred solution of the p-chlorobenzenesulfonyl chloride in chloroform. After the addition, the solution is stirred for 1 hour at room temperature and maintained for about 1 hour at room temperature. The chloroform is evaporated, and the residue is rubbed under ether. The resulting solid is taken up in acetonitrile, diluted with ether, rubbed and stored at a reduced temperature for several days, yielding 21.2 g of material, melting point 156°-158° C. Recrystallization from 130 ml of isopropanol yields 17 g of the title compound, melting point 163°-165° C.

WORKUP

后处理

  1. additionAfter the addition
  2. temperaturemaintained for about 1 hour at room temperature
  3. customThe chloroform is evaporated
  4. additiondiluted with ether
  5. waitstored at a reduced temperature for several days