反应详情

A mixture containing 16.32 g (0.08 mol) of 7-methyl-4-oxo-4H-pyrido[1,2-a]pyrimidine-3-carboxylic acid and 12.4 ml (0.088 mol) of triethylamine in 480 ml of chloroform is cooled below -10° C. by ice-salt. A solution of 6.5 ml (0.08 mol) of methyl chloroformate dissolved in 40 ml of chloroform is dropped to the above mixture at -18° C. during 20 minutes. After stirring for 5 minutes, 5.2 g (0.088 mol) of propylamine dissolved in 80 ml of chloroform are dropped to the above solution at -18° C. during 60 minutes. The reaction mixture is stirred at -10° C. for 1 hour, then allowed to stand overnight under cooling by ice. For working up, the reaction mixture is washed 3 times with 150 ml of 5% sodium hydrogen carbonate solution each, then 3 times with 150 ml of water each. The organic phase is dried over anhydrous sodium sulfate, filtered and evaporated to obtain 17.5 g (89.2%). of the named compound as yellow crystals after recrystallization from ethanol, m.p.: 126°-128° C.

1. additionis dropped to the above mixture at -18° C. during 20 minutes
2. additionare dropped to the above solution at -18° C. during 60 minutes
3. stirringThe reaction mixture is stirred at -10° C. for 1 hour
4. waitto stand overnight
5. temperatureunder cooling by ice
6. washthe reaction mixture is washed 3 times with 150 ml of 5% sodium hydrogen carbonate solution each, then 3 times with 150 ml of water each
7. dry with materialThe organic phase is dried over anhydrous sodium sulfate
8. filtrationfiltered
9. customevaporated
10. customto obtain 17.5 g (89.2%)
11. customof the named compound as yellow crystals after recrystallization from ethanol, m.p.: 126°-128° C.