反应详情

To a solution of the compound of Example 13 (1.17 g, 2.34 mmol) in methanol (20 mL) is added a solution of potassium hydroxide (0.987 g, 23.4 mmol) in water (10 mL) and the reaction stirred at reflux for 5 hr. The reaction is cooled to room temperature and the methanol removed under reduced pressure on a rotary evaporator. The aqueous residue is washed with ethyl acetate (2×25 mL) and then the pH is adjusted to 2-3 with 2N HCl. The aqueous phase is extracted with ether (2×50 mL) to yield the title compound (0.997 g, 88%).

1. temperatureat reflux for 5 hr
2. customthe methanol removed under reduced pressure on a rotary evaporator
3. washThe aqueous residue is washed with ethyl acetate (2×25 mL)
4. extractionThe aqueous phase is extracted with ether (2×50 mL)