반응 #4290

반응 방정식

3-chloropropylphenyl sulfone

isopropylamine

→

title compound

N-(1-Methylethyl)-3-(phenylsulfonyl)-1-propanamine hydrochloride

반응 조건

후처리

1. 1
   기타The isopropylamine was removed by rotary evaporation
2. 2
   기타the residue partitioned between chloroform and water
3. 3
   추출The chloroform layer was extracted with 1N sulfuric acid
4. 4
   추출extracted with chloroform
5. 5
   추출The combined chloroform extract
6. 6
   기타was evaporated
7. 7
   기타to give an oil

실험 절차

A solution of 66.55 g (0.3052 mole) of 3-chloropropylphenyl sulfone (prepared by reacting m-chloroperoxybenzoic acid and 3-chloropropyl phenylsulfide in methylene chloride) in 200 ml of isopropylamine was heated at 100° C. overnight in a bomb. The isopropylamine was removed by rotary evaporation and the residue partitioned between chloroform and water. The chloroform layer was extracted with 1N sulfuric acid. The acidic layer was made alkaline and extracted with chloroform. The combined chloroform extract was evaporated to give an oil, the free base of the title compound. The oil was converted to the hydrochloride salt by reacting with ethereal hydrogen chloride. Recrystallization of the precipitated salt from methanol-diethyl ether gave 48.04 g (65.3%) of white crystalline powder, m.p. 185°-186° C.

출처