反应详情

温度

130 °C

A mixture of 4-amino-8H-pyrido[2,3-d]pyrimidin-5-one (35 mg, 0.214 mmol), 2-chloromethyl-1-phenyl-1H-benzoimidazole (52 mg, 0.214 mmol), Cs2CO3 (105 mg, 0.321 mmol) and potassium iodide (4 mg, 0.021 mmol) in DMF (1 mL) was stirred for 3 h in a sealed tube at 130° C. Volatiles were then removed under reduced pressure and the residue suspended in DCM and filtered. The filtrate was purified by column chromatography (Si—PCC, gradient 0-10% 2M NH3/MeOH in DCM) and the resulting material was triturated with diethyl ether affording 111 as a pale yellow solid (28 mg, 36%). LCMS: RT 3.47 min [M+H]+ 369.1. 1H NMR (CDCl3, 400 MHz): δ 9.76 (1H, bs), 8.07 (1H, s), 7.82-7.77 (1H, m), 7.65 (1H, d, J=7.97 Hz), 7.50-7.44 (3H, m), 7.34-7.23 (4H, m), 7.14-7.09 (1H, m), 6.28 (1H, d, J=7.97), 5.86-5.78 (1H, m), 5.63 (2H, s)

1. customVolatiles were then removed under reduced pressure
2. filtrationfiltered
3. customThe filtrate was purified by column chromatography (Si—PCC, gradient 0-10% 2M NH3/MeOH in DCM)
4. customthe resulting material was triturated with diethyl ether affording 111 as a pale yellow solid (28 mg, 36%)