反应详情

To a solution of 2-amino-5-mesityl-3,7-dimethyl-3,7-dihydro-4H-pyrrolo[2,3-d]pyrimidin-4-one (55 mg, 0.18 mmol) and N,N-dimethylformamide (2 ml) was added sodium hydride (60% in oil, 24 mg, 0.60 mmol) at 0° C. and stirred for 0.5 hour. After stirring at room temperature for 0.5 hour, to the mixture was added a solution of 2-methoxyethylbromide (232 mg, 0.60 mmol) and N,N-dimethylformamide (1 ml) at 0° C. and stirred for 0.5 hour. After stirring at room temperature for 2 hours and heating under reflux for 2 hours, the mixture was diluted with water (20 ml) and extracted with ethyl acetate (50 ml×2). The extracts were combined, washed with brine, dried over sodium sulfate and concentrated in vacuo. The residue was purified by silica gel chromatography eluting with hexane/ethyl acetate (9:1) to give 15 mg (23%) of the title compound as an oil.

1. stirringAfter stirring at room temperature for 0.5 hour, to the mixture
2. stirringstirred for 0.5 hour
3. stirringAfter stirring at room temperature for 2 hours
4. temperatureheating
5. temperatureunder reflux for 2 hours
6. extractionextracted with ethyl acetate (50 ml×2)
7. washwashed with brine
8. dry with materialdried over sodium sulfate
9. concentrationconcentrated in vacuo
10. customThe residue was purified by silica gel chromatography
11. washeluting with hexane/ethyl acetate (9:1)