反应详情

温度

80 °C

To a solution of Intermediate 232B (0.15 g, 0.640 mmol) in ethanol (2 mL) and water (1 mL) was added NaOH (0.256 g, 6.40 mmol) and the reaction mixture was stirred at 80° C. for 12 h. The reaction mixture was concentrated under reduced pressure and the residue was acidified with an aqueous solution of 1.5N HCl and extracted with EtOAc (2×20 mL) The combined organic layer was dried over Na2SO4, filtered and the filtrate concentrated to afford Intermediate 232C as a yellow solid (90 mg, 68%). 1H NMR (300 MHz, DMSO-d6) δ ppm 12.20 (br. s., 1H), 2.11-1.94 (m, 2H), 1.91-1.55 (m, 5H), 1.34-1.14 (m, 2H), 1.09-0.96 (m, 6H).

1. concentrationThe reaction mixture was concentrated under reduced pressure
2. extractionextracted with EtOAc (2×20 mL) The combined organic layer
3. dry with materialwas dried over Na2SO4
4. filtrationfiltered
5. concentrationthe filtrate concentrated