反应详情

To a solution of 7-(1.4-dioxa-8-azaspiro[4.5]dec-8-yl)-8-fluoroquinoline (Example J, Step 2; 1.30 g) in tetrahydrofuran (60 mL) was added aq. 2N aqueous HCl (10 mL). The resulting mixture was stirred at room temperature for 18 hours and then heated at 60° C. for 5 hours. The reaction mixture was cooled to room temperature, poured into 1N aqueous NaOH and extracted with ethyl acetate. The combined organic layers were dried over anhydrous MgSO4, filtered and concentrated on a rotary evaporator. The crude product was purified by flash chromatography using hexane/acetone to give 0.89 g of the desired product as a yellow solid; MS (ES) m/z (relative intensity): 245 (M+H)+ (100).

1. temperatureheated at 60° C. for 5 hours
2. temperatureThe reaction mixture was cooled to room temperature
3. extractionextracted with ethyl acetate
4. dry with materialThe combined organic layers were dried over anhydrous MgSO4
5. filtrationfiltered
6. concentrationconcentrated on a rotary evaporator
7. customThe crude product was purified by flash chromatography