反应详情

A solution of N-(7-chloropyrazolo[1,5-a]pyrimidin-5-yl)-4-(2-hydroxypropan-2-yl)benzamide (2D, 50 mg, 151 mmol) and 2-methylpyrrolidine (26 mg, 0.302 mmol) in NMP (0.950 mL) was stirred at 85° C. overnight. After cooling to room temperature, the mixture was diluted with a few drops of DMSO and methanol, and was then purified by preparatory HPLC, 25-50% (MeCN/H2O gradient+0.01% TFA). Lyophilization of the combined fractions gave the titled compound as a orange solid (34 mg, 59%). 1H NMR (400 MHz, DMSO-d6) δ ppm 1.26 (d, J=6.06 Hz, 3 H) 1.45 (s, 6 H) 1.71-1.81 (m, 1 H) 1.90-2.01 (m, 1 H) 2.03-2.26 (m, 2 H) 3.75-3.91 (m, 1 H) 3.96-4.12 (m, 1 H) 4.96 (br. s., 1 H) 6.27 (d, J=2.27 Hz, 1 H) 6.98 (s, 1 H) 7.61 (d, J=8.34 Hz, 2 H) 7.91-8.09 (m, 3 H) 10.81 (s, 1 H). ESI-MS: m/z 380.3 (M+H)+.

1. customwas then purified by preparatory HPLC, 25-50% (MeCN/H2O gradient+0.01% TFA)