反应详情

温度

90 °C

To a solution of Intermediate 226A (150 mg, 0.942 mmol) in ethanol (10 mL) and H2O (10 mL) was added a 10% aqueous solution of NaOH (10 mL, 0.942 mmol) and the reaction mixture was stirred at 90° C. for 12 h. The reaction was then concentrated and the pH of the resultant residue was adjusted to 4 with a 1.5 N aq. solution of HCl and then extracted with EtOAc (3×10 mL). The combined organic layer was dried over Na2SO4, filtered and the filtrate evaporated under reduced pressure to afford Intermediate 226B as a yellow sticky liquid (100 mg, 60%). 1H NMR (400 MHz, chloroform-d) δ ppm 12.30 (bs, 1H), 2.40-2.57 (m, 5H), 1.23 (s, 6H).

1. concentrationThe reaction was then concentrated
2. extractionextracted with EtOAc (3×10 mL)
3. dry with materialThe combined organic layer was dried over Na2SO4
4. filtrationfiltered
5. customthe filtrate evaporated under reduced pressure