反应详情

温度

90 °C

The aforementioned mixture of amides 14a/14b (500 mg, 1.43 mmol) was suspended in glacial acetic acid (8 mL) and heated to 90° C. for 7 h. Most of the solvent was evaporated, and the yellow residue was suspended in Et2O. After being vigorously stirred for 20 min, the precipitate was filtered and washed with Et2O. Drying under hv gave 404 mg (85%) of 15 as a beige solid. Data of 15: Rf 0.80 (hexane/EtOAc 1:5). 1H NMR (300 MHz, DMSOd6): δ 3.76 (s, 3H), 4.14 (s, 3H), 4.34 (s, 3H), 7.14-7.17 (m, 1H), 7.48-7.55 (m, 3H), 8.25 (s, 1H). MS (ESI): m/z (rel intensity) 331 (98).

1. customMost of the solvent was evaporated
2. filtrationthe precipitate was filtered
3. washwashed with Et2O
4. customDrying under hv