反应详情

温度

85 °C

Methanesulfinic acid, sodium salt (11.75 g, 115.11 mmol) was added in one portion to 2-chloro-4-(iodomethyl)-6-[(3S)-3-methylmorpholin-4-yl]pyrimidine (37 g, 104.64 mmol), in acetonitrile (900 mL) and the resulting solution stirred at 85° C. for 24 hours. The organic layers were combined and washed with water (3×100 mL), dried over MgSO4, filtered, and the solvent was removed by evaporation to give the crude product as a dark brown oil, which solidifed (36 g). The crude solid was purified by flash silicachromatography, elution gradient 0 to 30% ethyl acetate in DCM, to give the desired material (22 g) as a cream solid which was identical to previous samples.

1. washwashed with water (3×100 mL)
2. dry with materialdried over MgSO4
3. filtrationfiltered
4. customthe solvent was removed by evaporation
5. customto give the crude product as a dark brown oil, which
6. customThe crude solid was purified by flash silicachromatography, elution gradient 0 to 30% ethyl acetate in DCM