反应详情

温度

60 °C

The product from step 1 (470 mg, 1.6 mmol, 1.0 equiv) was dissolved in MeOH (10 mL) and 2.5 M NaOH (2.5 mL) was added. The mixture was heated to 60° C. for three hours. When the reaction had cooled to room temperature, water and EtOAc were added. The phases were separated, and the aqueous layer was adjusted to pH 7 with 6N HCl. The aqueous phase was extracted with ethyl acetate. The organic extracts were dried over Na2SO4 and concentrated to dryness. The residue was azeotroped with hexanes to provide 335 mg (75%) of the title compound as a foamy white solid. MS (ES+) m/e 280 [M+H]+.

1. temperatureWhen the reaction had cooled to room temperature
2. customThe phases were separated
3. extractionThe aqueous phase was extracted with ethyl acetate
4. dry with materialThe organic extracts were dried over Na2SO4
5. concentrationconcentrated to dryness
6. customThe residue was azeotroped with hexanes