反应详情

Then, to a solution comprising of 100 ml of a tetrahydrofuran and 6.6 g (0.1 mole) of malononitrile was added 4.0 g (0.1 mole) of 60 wt% sodium hydride in nujol (paraffin oil) under ice-cooling, and, after adding thereto 17 g (0.1 mole) of 6-chloro-1,3-dimethyluracil, the mixture was stirred for 5 hours at room temperature. The reaction mixture thus obtained was mixed with 100 ml of water, neutralized with concentrated hydrochloric acid, and thereafter extracted with 200 ml of ethyl acetate. The extract was dried by anhydrous sodium sulfate, the solvent was distilled off under reduced pressure, and the crystals thus precipitated were collected by filtration to provide 12.9 g (63%) of 6-dicyanomethyl-1,3-dimethyluracil.

1. temperaturecooling
2. additionafter adding
3. customThe reaction mixture thus obtained
4. extractionextracted with 200 ml of ethyl acetate
5. dry with materialThe extract was dried by anhydrous sodium sulfate
6. distillationthe solvent was distilled off under reduced pressure
7. customthe crystals thus precipitated
8. filtrationwere collected by filtration