反应详情

温度

100 °C

To a solution of compound 27 (0.43 mmol) and NaOEt (2.15 mmol) in ethanol (2 mL) was added compound 28 (0.43 mmol). The reaction mixture was stirred at 100° C. overnight. The solvent was evaporated and water and AcOEt were added. The aqueous layer was acidified to pH˜4-5 by addition of 2.5M HCl. The organic layer was dried over Na2SO4, filtered, and concentrated under reduced pressure. The residue was purified by silica gel chromatography (eluent: DCM/MeOH 0 to 5%) to give compound 29 as a beige solid in 11% yield. MS (ESI, EI−): m/z=396.91 (MH−).

1. customThe solvent was evaporated
2. additionwater and AcOEt were added
3. additionThe aqueous layer was acidified to pH˜4-5 by addition of 2.5M HCl
4. dry with materialThe organic layer was dried over Na2SO4
5. filtrationfiltered
6. concentrationconcentrated under reduced pressure
7. customThe residue was purified by silica gel chromatography (eluent: DCM/MeOH 0 to 5%)