반응 #61666

반응 방정식

ethyl (2-methoxy-6-nitro-phenyl)-carbamate

SnCl2

→

ethyl (2-amino-6-methoxy-phenyl)-carbamate

용매

methanol

반응 조건

후처리

1. 1
   온도the mixture is refluxed for 3 hours
2. 2
   기타The reaction mixture is evaporated down
3. 3
   여과filtered
4. 4
   추출The aqueous phase is repeatedly extracted with dichloromethane
5. 5
   세척the combined organic phases are washed with sodium chloride solution
6. 6
   기타dried
7. 7
   기타evaporated down
8. 8
   기타The residue that crystallises out on standing

실험 절차

25.0 g (0.104 mol) ethyl (2-methoxy-6-nitro-phenyl)-carbamate are dissolved in 400 mL methanol. 116.4 g (0.516 mol) SnCl2 2H2O are added and the mixture is refluxed for 3 hours. The reaction mixture is evaporated down, combined with sodium carbonate solution and filtered. The aqueous phase is repeatedly extracted with dichloromethane and the combined organic phases are washed with sodium chloride solution, dried and evaporated down. The residue that crystallises out on standing is stirred with isopropanol. Yield: 13.0 g (59%); mass spectroscopy: [M+H]+=211.

출처