反应详情

To a stirred solution of methyl 3-amino-2-[(2′-cyanobiphenyl-4-yl)methylamino]benzoate (10 g) in pyridine (50 ml) was added dropwise methyl chloroformate (9.0 ml) under ice-cooling. The mixture was stirred at room temperature for 3 hours and concentrated. The residue was extracted with ethyl acetate. The extract was washed with water, dried and evaporated. The residue was recrystallized from ethyl acetate—hexane to afford pale yellow needles (10.5 g, 90%), m.p. 113-115° C.

1. temperaturecooling
2. concentrationconcentrated
3. extractionThe residue was extracted with ethyl acetate
4. washThe extract was washed with water
5. customdried
6. customevaporated
7. customThe residue was recrystallized from ethyl acetate—hexane