反应详情

温度

140 °C

Diethyl 1,4-dihydro-4-(3-hydroxypyridyl)-2,6-dimethyl-3,5-pyridine dicarboxylate (17.3 grams; 0.05 mole) was nearly dissolved in 250 ml toluene heated at 140° C. Diazabicyclo(5.4.0) undec-7-ene (8.3 grams; 8.2 ml; 0.05 mole) dissolved in 20 ml toluene was added and the reaction mixture refluxed for a period of 22 hours at 180° C. (bath temperature). The black solution was cooled and concentrated to afford 23.3 grams of a black paste. High pressure liquid chromatography (HPLC) using ethyl acetate yielded 8.3 grams of a yellow solid, m.p. 100°-150° C. Two recrystallizations from 2-propanol gave 4.5 grams (30%) of fluorescent yellow material, m.p. 150°-160° C.

1. additionwas added
2. temperaturethe reaction mixture refluxed for a period of 22 hours at 180° C. (bath temperature)
3. temperatureThe black solution was cooled
4. concentrationconcentrated
5. customto afford 23.3 grams of a black paste