反应详情

A solution of 4-(3-phenylpyrazolo[1,5-a]pyrimidin-6-yl)thiophene-2-carboxylic acid (5-3, 1.0 g, 3.11 mmol, 1 equiv) and oxalyl chloride (2.17 mL, 24.9 mmol, 8.00 equiv) in dichloromethane (400 mL) was stirred at 23° C. for 72 hours. The reaction mixture was concentrated to give 4-(3-phenylpyrazolo[1,5-a]pyrimidin-6-yl)thiophene-2-carbonyl chloride (5-4) as a yellow solid. 1H NMR (400 MHz, CDCl3) δ 8.89 (d, 1H, J=2.4 Hz), 8.79 (d, 1H, J=2.2 Hz), 8.50 (s, 1H), 8.22 (d, 1H, J=1.6 Hz), 8.05 (br d, 2H, J=7.8 Hz), 8.00 (d, 1H, J=1.6 Hz), 7.48 (br t, 2H, J=7.7 Hz), 7.31 (t, 1H, J=7.5 Hz).

1. concentrationThe reaction mixture was concentrated