反应详情

温度

100 °C

Benzyl chloroformate (7.5 g.) was added to a stirred solution of ethyl 6-amino-4-hydroxycinnolin-3-yl carboxylate (4.66 g.) in pyridine (75 ml.). The solution was stirred for 18 hours at room temperature and for 2 hours at 100° C. The solution was cooled and was poured onto a mixture of ice (500 g.) and 5N-hydrochloric acid (200 ml.). The pale solid which was precipitated was filtered off, washed with water, and recrystallised from a mixture of ethanol and water to give ethyl 6-benzyloxycarbonylamino-4-hydroxycinnolin-3-yl carboxylate, m.p. 250°-252° C.

1. temperatureThe solution was cooled
2. customThe pale solid which was precipitated
3. filtrationwas filtered off
4. washwashed with water
5. customrecrystallised from a mixture of ethanol and water