反应详情

Diethylbenzene Process: A mixture of 66.0 g of 2-amino-3-pyridinol, 220.0 g of diethyl ethoxymethylenemalonate, and 1.0 liter of diethylbenzene was heated so that the internal temperature reached 140° in 1 hour, was kept for 1 hour at 140°, then heated so that the temperature rose to 180° in 1 hour, and then kept 1 hour at 180°. During this entire heating period, 50 ml. of distillate was collected. The solution was allowed to cool spontaneously, was cooled at 0°, filtered, and the solid washed with diisopropyl ether to give 130.0 g of product, after drying at 56° in vacuo. The m.p. was 175°-177° and a mixture m.p. with the product isolated in (a) above was 175°-177°. The ir and pmr spectra of the two samples were superimposable. The yield was 93%.

1. temperaturewas heated so that the internal temperature
2. waitwas kept for 1 hour at 140°
3. temperatureheated so that the temperature
4. waitrose to 180° in 1 hour
5. waitkept 1 hour at 180°
6. temperatureDuring this entire heating period
7. distillationof distillate was collected
8. temperatureto cool spontaneously
9. temperaturewas cooled at 0°
10. filtrationfiltered
11. washthe solid washed with diisopropyl ether