反应详情

温度

80 °C

To a mixture of crude [2-(4-methoxy-5-nitro-pyrimidin-2-yloxy)-ethyl]-propyl-carbamic acid tert-butyl ester (1.76 g, 4.94 mmol) and 10% palladium on charcoal (200 mg) in water (15 ml) was slowly added a solution of ammonium formate (3.12 g, 49.44 mmol) in water (10 ml) at 80° C. After stirring for 1 h at 80° C. the mixture was filtered and concentrated under reduced pressure. The aqueous layer was extracted three times with dichloromethane. The combined organic layers were dried over MgSO4, filtered and the solvent was evaporated under reduced pressure. The residue was purified by silica gel chromatography with toluene/THF/MeOH (4:1:1)/2.5% triethylamine to give 720 mg (44.7%) of the title compound.

1. filtrationwas filtered
2. concentrationconcentrated under reduced pressure
3. extractionThe aqueous layer was extracted three times with dichloromethane
4. dry with materialThe combined organic layers were dried over MgSO4
5. filtrationfiltered
6. customthe solvent was evaporated under reduced pressure
7. customThe residue was purified by silica gel chromatography with toluene/THF/MeOH (4:1:1)/2.5% triethylamine