反应详情

To a solution of 2-amino-5-iodo-7-methyl-3,7-dihydro-4H-pyrrolo[2,3-d]pyrimidin-4-one (15.4 g, 53.1 mmol) in N,N-dimethylformamide (150 ml) was added sodium hydride (66% dispersion in oil, 1.93 g, 53.1 mmol) and iodomethane (3.31 ml, 53.1 mmol) at 0° C., and the mixture was stirred at the same temperature for 1 hour. The reaction mixture was diluted with water and extracted with ethyl acetate (×2) and ethyl acetate-tetrahydrofuran (×2). The combined organic layer was dried over sodium sulfate and concentrated in vacuo. The residue was purified by silica gel column chromatography eluting with a 50-100% hexane/ethyl acetate gradient mixture, and the desired fractions were concentrated in vacuo. The residual crystals were washed with diethyl ether to give 12.3 g (76%) of the title compound.

1. extractionextracted with ethyl acetate (×2) and ethyl acetate-tetrahydrofuran (×2)
2. dry with materialThe combined organic layer was dried over sodium sulfate
3. concentrationconcentrated in vacuo
4. customThe residue was purified by silica gel column chromatography
5. washeluting with a 50-100% hexane/ethyl acetate gradient mixture
6. concentrationthe desired fractions were concentrated in vacuo
7. washThe residual crystals were washed with diethyl ether