反应详情

A mixture prepared from 4-[[(dimethylamino)methylene]amino]-3-pyridinol (5.2 g), triethylamine (4.8 mL), piperidine carbonyl chloride (4.89 mL) and benzene (173 mL) was refluxed for a half hour, cooled, poured directly onto a silica column and eluted with 5% Et3N/ethyl acetate to yield 7.55 g of product. Recrystallization from ethyl acetate and drying under high vacuum for 2 hours yielded 5.5 g of crystals, m.p. 90°-91 ° C.

1. temperaturewas refluxed for a half hour
2. temperaturecooled
3. additionpoured directly onto a silica column
4. washeluted with 5% Et3N/ethyl acetate