反应详情

To 2-mercapto-4-methylpyrimidine·HCl (50.0 g, 0.307 mole) in toluene (750 mL), under argon, was added diisopropylethylamine (80.0 mL, 0.461 mole) followed by N,N-dimethylformamide dimethyl acetal (100 mL) and the mixture heated to reflux for 4 hours. Upon cooling, the reaction was concentrated in vacuo to an oil, dissolved in ether (400 mL), and washed with water (2×50 mL). The organic extract was dried over anhydrous sodium sulfate, filtered and concentrated to an oil which was vacuum distilled to give 2-methylthio-4-methylpyrimidine (36.4 g) as an oil.

1. temperaturethe mixture heated
2. temperatureto reflux for 4 hours
3. temperatureUpon cooling
4. concentrationthe reaction was concentrated in vacuo to an oil
5. dissolutiondissolved in ether (400 mL)
6. washwashed with water (2×50 mL)
7. extractionThe organic extract
8. dry with materialwas dried over anhydrous sodium sulfate
9. filtrationfiltered
10. concentrationconcentrated to an oil which
11. distillationdistilled