反应详情

To a solution of acid 4 (0.74 g, 2 mmol) in 10 mL of EtOH and 10 mL of 1,4-dioxane was added diphenylphosphonylazide (0.52 mL, 2.4 mmol) followed by Et3N (0.34 mL, 2.4 mmol). The reaction mixture was refluxed overnight. After cooling the reaction mixture to room temperature, EtOAc and water were added. The organic layer was separated, washed with brine, dried over MgSO4 and concentrated in vacuo. The residue was purified by column chromatography to give the titled compound (0.48 g, 62%) as a white solid. mp 120.9-127.5° C. 1H NMR (300 MHz, DMSO-d6): δ 10.30 (s, 1H), 7.79 (d, J=8 Hz, 2H), 7.50-7.34 (m, 7H), 7.33-7.25 (m, 2H), 6.74 (s, 1H), 4.14 (q, J=7 Hz, 2H), 1.24 (t, J=7 Hz, 3H).

1. temperatureThe reaction mixture was refluxed overnight
2. customThe organic layer was separated
3. washwashed with brine
4. dry with materialdried over MgSO4
5. concentrationconcentrated in vacuo
6. customThe residue was purified by column chromatography