反应详情

Tert-butylamine (II, 6.23 ml) is slowly added to 2,4,6-trichloropyrimidine (I, 10.0 g) at -20° (temp. rose to -14°). Diisopropylethylamine (9.50 ml) is added and the mixture is stirred at 20°-25° for 72 hours. Basic workup (ethyl acetate, 1N potassium bicarbonate, magnesium sulfate) and purification by flash chromatography eluting with hexane/ethyl acetate (9/1), pooling and concentrating the desired fractions gives the title compound, mp 192°-193°; NMR (CDCl3) 6.29, 1.44δ.

1. customBasic workup (ethyl acetate, 1N potassium bicarbonate, magnesium sulfate) and purification by flash chromatography
2. washeluting with hexane/ethyl acetate (9/1)
3. concentrationconcentrating the desired fractions