反应详情

A mixture of 21.7 g of t-butylamine in 100 mL of tetrahydrofuran is cooled to about -40° and treated over about 15 min with 170 mL of 1.6M n-butyllithium in hexane. The mixture is warmed to 0° for 2 hr, then recooled to -40° and treated over 30 min with a mixture of 25 g of 4-chloro-2, 6-di-1-pyrrolidinylpyrimidine and 50 mL of tetrahydrofuran. The mixture is allowed to warm to 20°-25° and is stirred for 16-18 hr. Water (50 mL) is then added and the mixture is concentrated under reduced pressure. The residue is partitioned between methylene chloride and aqueous 10% sodium bicarbonate. The organic phase is washed with saline, dried over anhydrous sodium sulfate and concentrated. Chromatography (silica gel, 5% ethyl acetate/hexane) gives the title compound, NMR (CDCl3) 4.78, 4.25, 3.53-3.49, 3.40, 1.93-1.86 and 1.41 6.

1. temperatureis cooled to about -40°
2. temperatureThe mixture is warmed to 0° for 2 hr
3. customrecooled to -40°
4. temperatureto warm to 20°-25°
5. concentrationthe mixture is concentrated under reduced pressure
6. customThe residue is partitioned between methylene chloride and aqueous 10% sodium bicarbonate
7. washThe organic phase is washed with saline
8. dry with materialdried over anhydrous sodium sulfate
9. concentrationconcentrated