反应详情

A mixture of 4-amino-3-pyridinol (3.0 g), N,N-diisopropylformamide dimethyl acetal (9.54 g) and 15 ml dry toluene was stirred at room temperature for 18 hours and thereafter heated to 60°-70° C. After 90 minutes, the mixture was cooled to room temperature, concentrated in vacuo and chromatographed on silica using 10:90 CH3OH/ethyl acetate as an eluent. The fractions containing the desired product were combined and concentrated to a thick oil, which solidified on refrigeration. This solid (5.3 g) was triturated with hexane three times to provide the product as a white solid, m.p. 77°-79° C.

1. temperatureheated to 60°-70° C
2. waitAfter 90 minutes
3. temperaturethe mixture was cooled to room temperature
4. concentrationconcentrated in vacuo
5. customchromatographed on silica using 10:90 CH3OH/ethyl acetate as an eluent
6. additionThe fractions containing the desired product
7. concentrationconcentrated to a thick oil, which
8. customThis solid (5.3 g) was triturated with hexane three times