反应详情

To a solution of dimethyl 5-phenoxyisophthalate (0.143 g, 0.50 mmol) in toluene (12 mL) was added drop-wise a solution of Red-A1 (60% in toluene, 0.673 mL, 2.0 mmol) and 1-methylpiperazine (0.243 mL, 2.2 mmol) in THF at 5° C., and the resulting mixture was stirred for 2 h. The reaction was quenched with H2O (4 mL), and then extracted with EtOAc (20 mL). The organic layer was washed with H2O (10 mL), dried over anhydrous Na2SO4, and then concentrated under reduced pressure. Purification by flash column chromatography (10% EtOAc/hexanes) afforded the desired product (0.094 g, 83%) as a white solid. 1H NMR (300 MHz, CDCl3) δ ppm 10.04 (s, 2H), 8.08 (s, 1H), 7.72 (t, J=1.5 Hz, 2H), 7.46-7.40 (m, 2H), 7.28-7.24 (m, 1H), 7.09-7.06 (m, 2H).

1. customThe reaction was quenched with H2O (4 mL)
2. extractionextracted with EtOAc (20 mL)
3. washThe organic layer was washed with H2O (10 mL)
4. dry with materialdried over anhydrous Na2SO4
5. concentrationconcentrated under reduced pressure
6. customPurification by flash column chromatography (10% EtOAc/hexanes)