反应详情

温度

25 °C

In an appropriate microwave vessel, a solution of 56 (0.129 g; 0.35 mmol) in dioxane (2 mL) at 25° C. was added aqueous sodium hydroxide (1.5 mL; 3.0 mmol; 2M). The vessel was sealed and brought to 110° C. for 10 minutes via the Biotage Initiator Microwave Synthesizer. Upon cooling to 25° C., the mixture was diluted with water (10 mL) and washed with diethyl ether (5 mL). The aqueous layer was treated with concentrated hydrochloric acid to pH 1 and extracted with dichloromethane (2×20 mL). The organic layers were combined, washed with water (5×25 mL), dried over magnesium sulfate, filtered, and concentrated under reduced pressure to yield the title product (0.54 g).

1. customThe vessel was sealed
2. washwashed with diethyl ether (5 mL)
3. additionThe aqueous layer was treated with concentrated hydrochloric acid to pH 1
4. extractionextracted with dichloromethane (2×20 mL)
5. washwashed with water (5×25 mL)
6. dry with materialdried over magnesium sulfate
7. filtrationfiltered
8. concentrationconcentrated under reduced pressure