反应详情

温度

50 °C

To a stirred solution of Compound 3 (70 mg, 0.175 mmol) in chloroform (15 mL) was added trifluoroacetic acid (3 mL) and heated to 50° C. overnight. The reaction was evaporated and diluted with water; pH was adjusted to 8-10 with sodium carbonate solution. The aqueous phase was extracted with dichloromethane twice (2×25 mL). The organic layer was dried over sodium sulphate and concentrated to get the crude, which was passed through 100-200 mesh silica gel eluting the EXAMPLE 1 at 60% ethyl acetate in hexane as pale yellow colour solid. MS-ES+ 277.9, 1H NMR (400 MHz, DMSO-D6-D6) 4: 13.29 (s, 1H), 10.29 (s, 1H), 8.74 (d, 1H), 8.40 (d, 1H), 8.03 (s, 1H), 7.69 (m, 1H), 7.43 (m, 2H), 6.44 (m, 1H), 6.26 (dd, 1H), 5.78 (dd, 1H), 2.55 (s, 3H).

1. customThe reaction was evaporated
2. additiondiluted with water
3. extractionThe aqueous phase was extracted with dichloromethane twice (2×25 mL)
4. dry with materialThe organic layer was dried over sodium sulphate
5. concentrationconcentrated
6. customto get the crude, which