反应详情

温度

80 °C

A solution of 28-h (3.8 g, 7.4 mmol) in 25 ml of dioxane was treated with 7.2 ml of 3N NaOH and heated at 80° C. for one hour. The mixture was cooled to room temperature and then concentrated under vacuum and the residue was diluted with water and washed with ethyl acetate. The aqueous layer was acidified with conc. HCl to pH=1 and the resulting solid was collected via filtration to give compound 28-1 (1.4 g of crude), which was further purified via prep-HPLC (150 mg, 4%). 1H NMR (300 MHz, CD3OD): δ 8.72 (s, 1H), 8.17 (s, 1H), 7.81 (m, 3H), 7.43 (m, 2H), 7.20 (m, 2H), 7.11 (m, 2H), 6.71 (s, 1H), 1.65 (d, 3H). (M+H)+=486.0.

1. temperatureThe mixture was cooled to room temperature
2. concentrationconcentrated under vacuum
3. additionthe residue was diluted with water
4. washwashed with ethyl acetate
5. filtrationthe resulting solid was collected via filtration