反应详情

To 50 mg of 1-{2-[6-amino-8-(3-fluorophenyl)-9-methyl-9H-2-purinyl]-1-ethynyl}-1-cyclopentanol were added 3.0 ml of allyl alcohol and 1.0 ml of 5M NaOH, the mixture was stirred at room temperature for 10 minutes, 1.0 ml of THF was added thereto and the mixture was stirred again at room temperature for 15 hours and 40 minutes. The solvent was evaporated and then 200 ml of ethyl acetate and water (1:1) were added and an extraction was carried out. The aqueous layer was extracted with 100 ml of ethyl acetate again and the all organic layers were combined and washed with water and with brine once each. The organic layer was dried over anhydrous sodium sulfate and the solvent was evaporated. The resulting residue was purified by a p-TLC (CH2Cl2:MeOH=10:1), the resulting yellowish white crystals were suspended in diethyl ether and the suspension was filtered to give 217 mg of the title compound as white crystals. The yield was 36%.

1. stirringthe mixture was stirred again at room temperature for 15 hours and 40 minutes
2. customThe solvent was evaporated
3. addition200 ml of ethyl acetate and water (1:1) were added
4. extractionan extraction
5. extractionThe aqueous layer was extracted with 100 ml of ethyl acetate again
6. washwashed with water and with brine once each
7. dry with materialThe organic layer was dried over anhydrous sodium sulfate
8. customthe solvent was evaporated
9. customThe resulting residue was purified by a p-TLC (CH2Cl2:MeOH=10:1)
10. filtrationthe suspension was filtered