反应详情

温度

25 °C

A mixture of 4,6-dichloro-2-methylpyrimidine (11.5 g, 70.6 mmol, Aldrich) and sodium methanethiolate (5.93 g, 85 mmol, Aldrich) in toluene (50 mL) was stirred at 25° C. for 24 h. The reaction mixture was concentrated in vacuo. The residue was diluted with EtOAc, washed with brine, and dried over Na2SO4. The crude product was purified by recrystallization from hexane to give 4-chloro-2-methyl-6-(methylthio)pyrimidine (5.5 g, 31.5 mmol, 44.6% yield) as white crystals. 1H NMR (400 MHz, CDCl3) δ 7.01 (s, 1H); 2.64 (s, 3H); 2.56 (s, 3H). m/z (ESI, +ve ion) 175 (M+H)+.

1. concentrationThe reaction mixture was concentrated in vacuo
2. additionThe residue was diluted with EtOAc
3. washwashed with brine
4. dry with materialdried over Na2SO4
5. customThe crude product was purified by recrystallization from hexane