반응 #55447

반응 방정식

N-[2-(3,4-dibenzyloxyphenyl)ethyl]-2-(N-benzyloxycarbonyl-p-chloroanilino)acetamide

phosphorus oxychloride

→

1-(N-benzyloxycarbonyl-p-chloroanilinomethyl)-6,7-dibenzyloxy-3,4-dihydroisoquinoline

수율 197.4%

용매

benzene

반응 조건

후처리

1. 1
   온도was refluxed for four hours
2. 2
   농축The reaction mixture was concentrated to dryness under reduced pressure and to the residue
3. 3
   workup.ADDITIONwas added a diluted aqueous ammonia solution
4. 4
   추출the mixture was extracted with ethyl acetate
5. 5
   세척The extract was washed with water
6. 6
   기타dried
7. 7
   workup.DISTILLATIONthe solvent was distilled off

실험 절차

A mixture of N-[2-(3,4-dibenzyloxyphenyl)ethyl]-2-(N-benzyloxycarbonyl-p-chloroanilino)acetamide (7.3 g), phosphorus oxychloride (2.3 g) and anhydrous benzene (73 ml) was refluxed for four hours. The reaction mixture was concentrated to dryness under reduced pressure and to the residue was added a diluted aqueous ammonia solution, and then the mixture was extracted with ethyl acetate. The extract was washed with water and dried, and the solvent was distilled off to give 1-(N-benzyloxycarbonyl-p-chloroanilinomethyl)-6,7-dibenzyloxy-3,4-dihydroisoquinoline (7.0 g).

출처