反应详情

温度

0 °C

1.0 g of 6-trifluoromethyl-2,4(1H,3H)-pyrimidinedione was added to 10 ml of dimethylformamide, followed by addition of 0.65 g of sodium hydride (purity: 55%) with stirring at 0° C. The mixed solution was stirred at room temperature for 30 minutes, then cooled to 0° C. and added dropwise with a 5 ml dimethylformamide solution of 1.89 g of 2-chloro-3,5-dinitrobenzotrifluoride. After the solution was further stirred at room temperature for 3 hours, the solvent was distilled away under reduced pressure. After addition of cooled dilute hydrochloric acid thereto, the residue was extracted with 100 ml of ethyl acetate. The obtained organic layer was dried over anhydrous sodium sulfate and then the solvent was distilled away under reduced pressure to form a crude product. This crude product was recrystallized from a mixed solvent of chloroform and petroleum ether to obtain 0.77 g of the objective compound.

1. stirringThe mixed solution was stirred at room temperature for 30 minutes
2. temperaturecooled to 0° C.
3. stirringAfter the solution was further stirred at room temperature for 3 hours
4. distillationthe solvent was distilled away under reduced pressure
5. additionAfter addition
6. temperatureof cooled dilute hydrochloric acid
7. extractionthe residue was extracted with 100 ml of ethyl acetate
8. dry with materialThe obtained organic layer was dried over anhydrous sodium sulfate
9. distillationthe solvent was distilled away under reduced pressure
10. customto form a crude product
11. customThis crude product was recrystallized from a mixed solvent of chloroform and petroleum ether