反应详情

温度

80 °C

To a suspension of 2-amino-7-methyl-3,7-dihydro-4H-pyrrolo[2,3-d]pyrimidin-4-one (4.82 g, 29.4 mmol) in pyridine (45 ml) was added pivaloyl chloride (11.6 ml, 94.0 mmol) at 0° C., and the mixture was stirred at 80° C. for 2 hours. After cooling, the reaction mixture was diluted with water and extracted with ethyl acetate (×1). The organic layer was washed with water (×1) and brine (×1), dried over sodium sulfate and concentrated in vacuo. The residual solids were suspended in methanol (45 ml), and concentrated aqueous ammonia (10 ml) was added at 0° C. The suspension was stirred at the same temperature for 30 minutes, before addition of water. After stirring at 0° C. for 2 hours, the resulting crystals were collected by filtration and washed with water to give 5.46 g (75%) of the title compound.

1. temperatureAfter cooling
2. extractionextracted with ethyl acetate (×1)
3. washThe organic layer was washed with water (×1) and brine (×1)
4. dry with materialdried over sodium sulfate
5. concentrationconcentrated in vacuo
6. additionconcentrated aqueous ammonia (10 ml) was added at 0° C
7. stirringThe suspension was stirred at the same temperature for 30 minutes, before addition of water
8. stirringAfter stirring at 0° C. for 2 hours
9. filtrationthe resulting crystals were collected by filtration
10. washwashed with water