反应详情

To a solution of NaOH (7.46 g, 186.4 mmol) in water (120 mL), 4-methylpyrimidine-2-thiol hydrochloride (13.78 g, 84.7 mmol) was added and subsequently iodomethane (13.23 g, 93.2 mmol) was added dropwise under argon atmosphere. It was stirred at room temperature for 2 h. It was extracted with CH2Cl2 (×2). The organic phase was dried over Na2SO4 and concentrated to dryness. The crude product obtained was purified by chromatography on silica gel using hexane-EtOAc mixtures of increasing polarity as eluent, to afford 10.26 g of the desired compound (yield: 86%).

1. extractionIt was extracted with CH2Cl2 (×2)
2. dry with materialThe organic phase was dried over Na2SO4
3. concentrationconcentrated to dryness
4. customThe crude product obtained
5. customwas purified by chromatography on silica gel
6. temperatureof increasing polarity as eluent