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