反应详情

0.14 mole (15.7 g) of ethyl chloroformate is slowly added dropwise to 0.13 mole (33 g) of 5-amino -2-(benzyloxycarbonylamino)phenol (prepared in Example 1, 2nd stage) and 7.1 g of calcium carbonate in 100 ml of dioxane brought to 80° C. The mixture is heated for a further 20 minutes after the addition is complete. The reaction mixture is filtered while hot in order to remove the inorganic salts. The expected product is precipitated by diluting the cooled filtrate with ice-cold water. When recrystallized from ethyl acetate, it melts at 190° C.

1. custombrought to 80° C
2. temperatureThe mixture is heated for a further 20 minutes
3. additionafter the addition
4. filtrationThe reaction mixture is filtered while hot in order
5. customto remove the inorganic salts
6. customThe expected product is precipitated
7. additionby diluting the cooled filtrate with ice-cold water
8. customWhen recrystallized from ethyl acetate, it melts at 190° C.