反应详情

温度

135 °C

A mixture of 4,6-diamino-2-ethylmercaptopyrimidine (9.95 g) and diethyl ethoxymethylene malonate (13.77 g) at 165° C. was stirred for 40 minutes, cooled to 135° C., stirred for 60 minutes, cooled to 25° C., and added to refluxing ethanol (700 mL). This mixture was treated with decolorizing carbon (NORIT®) stirred for 30 minutes, cooled, filtered, concentrated to 300 mL, heated until homogeneous, cooled, treated with water until cloudy, stored at 0° C. for 18 hours, and filtered. 1H NMR (300 MHz, DMSO-d6) δ 10.41 (d, 1H), 8.96 (d, 1H), 6.98 (s, 2H), 5.97 (s, 1H), 4.21 (q, 2H), 4.12 (q, 2H), 2.43 (s, 3H), 1.26 (t, 3H), 1.23 (t, 3H).

1. stirringstirred for 60 minutes
2. temperaturecooled to 25° C.
3. additionadded
4. additionThis mixture was treated with decolorizing carbon (NORIT®)
5. stirringstirred for 30 minutes
6. temperaturecooled
7. filtrationfiltered
8. concentrationconcentrated to 300 mL
9. temperatureheated until homogeneous,
10. temperaturecooled
11. additiontreated with water until cloudy
12. waitstored at 0° C. for 18 hours
13. filtrationfiltered