反应详情

A mixture prepared from 4-[[(dimethylamino)methylene]amino]-3-pyridinol N,N-dimethylcarbamate (7.4 g), trifluoroacetic acid (30 mL) and water (15 mL) was refluxed for a half hour. The reaction mixture was concentrated, filtered over a pad of basic alumina (CH2Cl2, 30% ethyl acetate/CH2Cl2, ethyl acetate), recrystallized from methanol/diethyl ether, and dried under high vacuum and refluxing ethanol to yield 4.97 g of microcrystals, m.p. 159°-160° C.

1. temperaturewas refluxed for a half hour
2. concentrationThe reaction mixture was concentrated
3. filtrationfiltered over a pad of basic alumina (CH2Cl2, 30% ethyl acetate/CH2Cl2, ethyl acetate)
4. customrecrystallized from methanol/diethyl ether
5. customdried under high vacuum
6. temperaturerefluxing ethanol
7. customto yield 4.97 g of microcrystals, m.p. 159°-160° C.