反应详情

温度

50 °C

To a solution of the product of Example 24b (7.8 g, 11.6 mmol) in tetrahydrofuran (40 ml)/ethanol (40 ml) was added an aqueous lithium hydroxide solution (0.84 g of lithium hydroxide in 40 ml of H2O). The resulting mixture was heated to 50° C. for two hours and cooled to room temperature. The organic solvents were mostly removed under reduced pressure, and the resulting residue was acidified with 10% citric acid aqueous solution and extracted with ethyl acetate (200 ml). The organic layer was separated, washed with brine (200 ml), dried over anhydrous Na2SO4, filtered and concentrated under reduced pressure to give a light yellow solid, which was further dried in a vacuum oven at 45° C. for 18 h to afford 7.5 g of product 24c as a light yellow solid; MS-DCI/NH3: 643 (M+H)+.

1. temperaturecooled to room temperature
2. customThe organic solvents were mostly removed under reduced pressure
3. extractionextracted with ethyl acetate (200 ml)
4. customThe organic layer was separated
5. washwashed with brine (200 ml)
6. dry with materialdried over anhydrous Na2SO4
7. filtrationfiltered
8. concentrationconcentrated under reduced pressure
9. customto give a light yellow solid, which
10. customwas further dried in a vacuum oven at 45° C. for 18 h