반응 #55247

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N-[[2-[3-(4-Morpholinyl)propoxy]phenyl]methyl]benzeneethanamine

p-chlorobenzenesulfonyl chloride

p-chlorobenzenesulfonyl chloride

→

material

수율 172.0%

4-Chloro-N-[[2-[3-(4-morpholinyl)propoxy]phenyl]methyl]-N-(2-phenylethyl)benzenesulfonamide, hydrochloride

수율 172.0%

용매

chloroform

chloroform

chloroform

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후처리

1. 1
   workup.ADDITIONAfter the addition
2. 2
   온도maintained for about 1 hour at room temperature
3. 3
   기타The chloroform is evaporated
4. 4
   workup.ADDITIONdiluted with ether
5. 5
   workup.WAITstored at a reduced temperature for several days

실험 절차

N-[[2-[3-(4-Morpholinyl)propoxy]phenyl]methyl]benzeneethanamine (14 g, 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.

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