反应详情

温度

80 °C

The product of step D, 1-1-d, (500 mg, 1.05 mmol) was dissolved in 10 mL of dioxane and treated with 2 mL of 5N NaOH. The mixture was heated at 80° C. for 30 min. The mixture was then diluted with water and extracted with dichloromethane. The aqueous layer was adjusted to pH=5 with AcOH and evaporated to dryness. The residue was used for prep-HPLC to afford the product, 1-1, (130 mg, 28%). 1H NMR (300 MHz, DMSO-d6): δ 10.38 (br, 1H), 8.79 (s, 1H), 8.48 (s, 1H), 8.18 (s, 1H), 7.37 (m, 10H), 6.29 (d, 1H), 1.63 (d, 3H). (M+H)+ =450.1.

1. extractionextracted with dichloromethane
2. customevaporated to dryness
3. customto afford the product, 1-1, (130 mg, 28%)