反应详情

温度

10 °C

A 500 mL multi-neck flask with overhead stirrer, thermocouple and addition funnel was charged with 2-cyclopropyl-1,6-dihydro-6-oxo-4-pyrimidinecarboxylic acid (36 g, 0.20 mol), water (70 mL) and 50 wt. % aqueous NaOH (14.4 g, 0.18 mol). The mixture was stirred at 10° C., and 10.3% aqueous NaOCl (160 g, 0.22 mol) was added over 1.5 h with cooling to maintain the reaction mixture at 10° C. The mixture was cooled to 5° C., and sodium sulfite was added until KI-starch paper gave negative test results. Hydrochloric acid (37 wt. % in water, 44.3 g, 0.443 mol) was added at 5° C. over about 30 minutes to lower the pH to 0.8. The mixture was filtered, and the collected solid was washed with cold 1 N HCl (20 mL), and dried to constant weight in a vacuum-oven at 50° C. to give 40.9 g (95% yield) of the title compound as a solid melting at 189-190° C.

1. additionA 500 mL multi-neck flask with overhead stirrer, thermocouple and addition funnel
2. temperaturewith cooling
3. temperatureto maintain the reaction mixture at 10° C
4. temperatureThe mixture was cooled to 5° C.
5. customgave negative test
6. customresults
7. filtrationThe mixture was filtered
8. washthe collected solid was washed with cold 1 N HCl (20 mL)
9. customdried to constant weight in a vacuum-oven at 50° C.