反应详情

To 5.4 g of 5-tert-butoxycarbonylamino-2-chloro-isonicotinic acid in 50 mL of methanol and 100 mL of chloroform was at 0° C. was added 15 mL of 2 M (trimethylsilyl)diazomethane in hexanes. After allowing the reaction to warm to ambient temperature and stirring for 2 hours, the solvents were removed and the crude product purified by passing through a plug of silica gel with chloroform. The product was then recrystallized from hexanes to give 5.8 g (100%) of 5-tert-butoxycarbonylamino-2-chloro-isonicotinic acid, methyl ester: mp=90-96° C. (decomposed); mass spectrum (m/e): M+H 287.1.

1. customwas at 0° C.
2. customthe reaction
3. customthe solvents were removed
4. customthe crude product purified
5. customThe product was then recrystallized from hexanes