反应详情

2,4,6-Trichloropyrimidine (I, 30 g) is added to a suspension of methylamine hydrochloride (II, 10 g) in THF (250 ml). The mixture is cooled to -6° and diisopropylethylamine (55 ml) is added slowly. The mixture is stirred for 3 days at 20°-25° and then is concentrated under reduced pressure. The residue is absorbed on silica gel (75 g) with ethyl acetate/methylene chloride (1/1) and applied to a silica gel (1 kg) column packed in ethyl acetate/hexane (1/1). Elution is performed with ethyl acetate/hexane (1/1) collecting 500 ml fractions. The appropriate fractions (8-14) are pooled and concentrated to give the title compound, NMR (CDCl3) 6.29, 6.2 and 2.9δ.

1. temperatureThe mixture is cooled to -6°
2. concentrationis concentrated under reduced pressure
3. customThe residue is absorbed on silica gel (75 g) with ethyl acetate/methylene chloride (1/1)
4. washElution
5. customcollecting 500 ml fractions
6. concentrationconcentrated