反应详情

温度

0 °C

A 0.57M solution of diazomethane in diethyl ether (108 cc.) is added to a suspension of 7-carboxymethoxyimino-7H-indolizino[5,6,7-ij]isoquinoline (15 g.) in dimethylformamide (150 cc.) cooled to 0° C. The mixture is kept at between 0° and 5° C. for 3 hours and is then allowed to return to a temperature of about 20° C. Water (450 cc.) is then added, the mixture is cooled in an ice-water bath and the yellow crystals thus obtained are filtered off. After drying, the crude methyl ester (14.17 g.) is obtained. After recrystallisation from ethyl acetate (280 cc.), the 7-methoxycarbonylmethoxyimino-7H-indolizino[5,6,7-ij]isoquinoline obtained melts at 148 ° C. with decomposition.

1. customto return to a temperature of about 20° C
2. temperaturethe mixture is cooled in an ice-water bath
3. customthe yellow crystals thus obtained
4. filtrationare filtered off
5. customAfter drying
6. customthe crude methyl ester (14.17 g.) is obtained
7. customAfter recrystallisation from ethyl acetate (280 cc.)