反应详情

温度

130 °C

3-(2-amino-4-methyl-phenylsulfanyl)-phenol (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 a solid in the acetic acid solvent appeared which was collected by filtration to provide the title compound as an acetic acid salt (78 mg, 68%). 1H NMR (300 MHz, DMSO-D6) δ ppm: 0.95 (t, J=7.3 Hz, 3H), 1.79 (m, 2H), 1.88 (s, 6H), 2.40 (s, 3H), 2.88 (t, J=7.6 Hz, 2H), 6.57 (m, 3H), 7.00 (t, J=7.7 Hz, 1H), 7.13 (m, 1H), 7.26 (d, J=7.7 Hz, 1H), 7.38 (s, 1H), 7.51 (d, J=8.5 Hz, 1H), 8.50 (s, 1H), 8.70 (d, J=8.5 Hz, 1H); MS (ESI)+ m/z 403 (M+H)+.

1. filtrationwas collected by filtration