反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- additionAfter the addition
- temperaturemaintained for about 1 hour at room temperature
- customThe chloroform is evaporated
- additiondiluted with ether
- waitstored at a reduced temperature for several days