반응 #54280

반응 방정식

1-(3,4-methylenedioxyphenyl)-2-chloroethanol

ethylamine

→

1-(3,4-methylenedioxyphenyl)-2-ethylaminoethanol hydrochloride

용매

ethanol

반응 조건

후처리

1. 1
   온도After cooling
2. 2
   workup.DISTILLATIONthe ethanol and excess ethylamine are distilled off under reduced pressure
3. 3
   추출The residue is extracted with 100 ml
4. 4
   세척of 1N HCl and the extract is washed twice with 100 ml
5. 5
   추출The hydrochloric acid extract solution
6. 6
   추출the liberated oil is extracted with ether
7. 7
   추출The ether extract
8. 8
   기타is dried
9. 9
   workup.ADDITIONan etherial hydrochloric acid solution is added
10. 10
    여과are filtered off
11. 11
    세척washed with ether
12. 12
    기타Upon recrystallization from isopropyl alcohol 7.8 g

실험 절차

19.5 g. of 1-(3,4-methylenedioxyphenyl)-2-chloroethanol are added to a solution of 170 g. of ethylamine in 200 ml. of cooled ethanol and the mixture is heated at 80° C. for 8 hours in an autoclave. After cooling, the ethanol and excess ethylamine are distilled off under reduced pressure. The residue is extracted with 100 ml. of 1N HCl and the extract is washed twice with 100 ml. of ether. The hydrochloric acid extract solution is made basic with 1N caustic soda and the liberated oil is extracted with ether. The ether extract is dried and an etherial hydrochloric acid solution is added thereto. The crystals which settle out on standing are filtered off and washed with ether. Upon recrystallization from isopropyl alcohol 7.8 g. of 1-(3,4-methylenedioxyphenyl)-2-ethylaminoethanol hydrochloride are obtained.

출처