反应详情

温度

100 °C

A suspension of 2-(2-(2-(2-chloro-5-methylpyrimidin-4-yl)ethyl)phenyl)acetamide (K6) (0.150 g, 0.518 mmol), 4-amino-1-(1-Boc-azetidin-3-yl)-1H-pyrazole (0.195 g, 0.777 mmol), Pd(OAc)2 (2.3 mg, 0.010 mmol), Cs2CO3 (0.506 g, 1.55 mmol) and Xantphos (11.9 mg, 0.021 mmol) in 1,4-dioxane (2 mL) was heated under microwave irradiation at 100° C. for 1.5 hours. 4-Amino-1-(1-Boc-azetidin-3-yl)-1H-pyrazole (65.0 mg, 0.259 mmol) was added and the mixture was heated for a further 1 hour at 100° C. The resulting mixture was adsorbed onto silica gel and purified using column chromatography (CombiFlash Rf, 12 g SiO2 cartridge, 0-5% MeOH in DCM) to give the title compound A120 as a light pink colored foam (0.050 g, 19%); 1H NMR (300 MHz, d4-MeOH) δ 8.06 (d, J=8.8 Hz, 2H), 7.66 (s, 1H), 7.16-7.27 (m, 4H), 5.12-5.21 (m, 1H), 4.39 (t, J=8.7 Hz, 2H), 4.25-4.30 (m, 2H), 3.65 (s, 2H), 3.32 (s, 1H), 3.10-3.16 (m, 2H), 2.95-3.00 (m, 2H), 2.10 (s, 3H), 1.48 (s, 9H). LCMS-B: rt 6.184 min; m/z 492 [M+H]+.

1. temperaturethe mixture was heated for a further 1 hour at 100° C
2. custompurified