반응 #5336

반응 방정식

compound

Methyl 2-[N-tert-butoxycarbonyl-N-(2'-carbamoylbiphenyl-4-yl)methylamino1-3-nitrobenzoate

HCl

→

needles

수율 73.0%

Methyl 2-(2'-carbamoylbiphenyl-4-yl)methylamino-3-nitrobenzoate

수율 73.0%

용매

methanol

반응 조건

후처리

1. 1
   온도was heated for 2 hours
2. 2
   온도under reflux
3. 3
   기타After removal of the solvent
4. 4
   추출the mixture was extracted with ethyl acetate
5. 5
   세척The extract was washed with water
6. 6
   건조dried over MgSO4
7. 7
   농축concentrated to dryness
8. 8
   기타The residue was purified by column chromatography on silica gel
9. 9
   기타the product was recrystallized from ethyl acetate - hexane

실험 절차

A mixture of the compound (2.8 g) obtained in Example (54b) in methanol (15 ml) and 1N-HCl (6 ml) was heated for 2 hours under reflux. After removal of the solvent, the residue was made alkaline with an aqueous solution of NaHCO3, and the mixture was extracted with ethyl acetate. The extract was washed with water, dried over MgSO4 and concentrated to dryness. The residue was purified by column chromatography on silica gel, and the product was recrystallized from ethyl acetate - hexane to afford yellow needles (1.6 g, 73%).

출처