反应详情

温度

90 °C

A mixture of 2,2-dimethylpropionic acid 2-{(S)-3-[2-((S)-2-aminopropionylamino)-5-fluorophenylamino]piperidin-1-yl}ethyl ester, (0.591 g, 1.45 mmol), 6-chloro-9-(tetrahydropyran-2-yl)-9H-purine (0.346 g, 1.45 mmol), and DIPEA (0.74 mL, 4.32 mmol) in n-butanol (7 mL) was stirred in a sealed vial at 90° C. for 16 h. After cooling to RT the volatiles were removed in vacuo and the resulting residue purified by column chromatography (Si—PCC, gradient 2-8% 2M NH3/MeOH in DCM) affording the title compound as a colourless gum (0.583 g, 66%). LCMS (Method J): RT 2.39 min [M+H]+ 611.

1. temperatureAfter cooling to RT the volatiles
2. customwere removed in vacuo
3. customthe resulting residue purified by column chromatography (Si—PCC, gradient 2-8% 2M NH3/MeOH in DCM)