反应详情

The 2-(2,6-dichloropyrimidin-4-ylamino)ethanesulfonic acid (III, EXAMPLE 97, 3.0 g) is dissolved in pyrrolidine (IV, 125 ml) and heated to reflux. Solvent evaporation gives a semisolid which is chromatographed on 155 g of silica gel eluting with chloroform/3.9M ammonia in methanol (7/3). An initial fraction of 150 ml is collected followed by 15 ml fractions. Fractions 8-18 contained the desired product. Solvent evaporation and drying under high vacuum gives a solid (a portion of which) is rechromatographed on 155 g silica gel and eluting with the same solvent system as described above. The appropriate fractions are pooled and concentrated to give the title compound, which is used in subsequent reactions without further purification.

1. temperatureheated to reflux
2. customSolvent evaporation
3. customgives a semisolid which
4. customis chromatographed on 155 g of silica gel eluting with chloroform/3.9M ammonia in methanol (7/3)
5. customAn initial fraction of 150 ml is collected
6. customSolvent evaporation
7. customdrying under high vacuum
8. customgives a solid (a portion of which)
9. customis rechromatographed on 155 g silica gel
10. washeluting with the same solvent system
11. concentrationconcentrated