反应详情

3-(1-((tert-butyldimethylsilyl)oxy)ethyl)-4-(morpholinomethyl)-1H-isochromen-1-one (Intermediate B59.3, 0.203 g, 0.503 mmol) was dissolved in THF (7 mL); TBAF (1.0 M solution in THF, 0.33 ml, 0.33 mmol) was added drop-wise and the resulting mixture was stirred at room temperature for 2 hrs. Water (10 ml) was added and the mixture was extracted twice with DCM; the combined organic layers were dried over sodium sulfate and evaporated to dryness. The crude was purified by reverse phase flash chromatography on C18 Biotage cartridge ((H2O:CH3CN=95:5 to 80:20, with 0.1% HCOOH) to afford the title compound (0.145 g). The product was used in the next step without further purifications.

1. extractionthe mixture was extracted twice with DCM
2. dry with materialthe combined organic layers were dried over sodium sulfate
3. customevaporated to dryness
4. customThe crude was purified by reverse phase flash chromatography on C18 Biotage cartridge ((H2O:CH3CN=95:5 to 80:20, with 0.1% HCOOH)