反应详情

温度

130 °C

The product from Example 7b (49 mg 0.231 mmol) and the product from Example 128A (50 mg, 0.231 mmol) were dissolved in acetic acid (1 mL) and heated to 130° C. for 1.5 hours. After cooling to room temperature and removal of the acetic acid solvent under vacuum methanol (3 mL) was added to the oil which caused a solid to form which was triturated with methanol to provide the title compound 80 mg, 78%). 1H NMR (300 MHz, DMSO-D6) δ ppm: 0.95 (t, J=7.4 Hz, 3H), 1.89 (m, 2H), 2.02 (s, 3H), 2.32 (s, 3H), 2.89 (t, J=7.5 Hz, 2H), 7.06 (s, 2H), 7.21 (t, J=8.5 Hz, 2H), 7.30 (s, 1H), 7.50 (d, J=8.8 Hz, 2H), 7.52 (m, 1H), 8.52 (s, 1H), 8.74 (d, J=7.7 Hz, 1H), 10.00 (s, 1H); MS (ESI)+ m/z 444 (M+H)+.

1. temperatureAfter cooling to room temperature
2. customremoval of the acetic acid solvent under vacuum methanol (3 mL)
3. additionwas added to the oil which
4. customto form which
5. customwas triturated with methanol