反应详情

温度

175 °C

A mixture of spray-dried KF (410 mg, 7.06 mmol), intermediate 11 (200 mg, 0.706 mmol) and catalytic amount of 18-crown-6 in dry DMSO (5 mL) was stirred at 170-180° C. for 30 min. Work-up of the reaction mixture as described in example 1 gave the product as a pale brown color solid (117 mg, 65%), mp 136-138° C. 1H NMR (400 MHz, DMSO-d6): 812.74 (1H, br s), 8.96 (1H, d, J=7.2 Hz), 8.21 (1H, d, J=9.6 Hz), 8.16 (1H, d, J=8.4 Hz), 7.82 (1H, t, J=7.6 Hz), 4.42 (1H, pentet, J=7.0 Hz), 1.38 (3H, d, J=7.2 Hz); LC-MS (negative ion mode): m/z 255 (M−H)−.