反应详情

温度

100 °C

A mixture of 2,2-dimethylpropionic acid 2-{(R)-3-[2-((S)-2-aminopropionylamino)-5-fluorophenylamino]piperidin-1-yl}ethyl ester (0.255 g, 0.62 mmol), 6-chloro-9-(tetrahydropyran-2-yl)-9H-purine (0.149 g, 0.62 mmol), and DIPEA (0.32 mL, 1.87 mmol) in n-butanol (4 mL) was stirred in a sealed vial at 100° C. for 2 h, then at 90° C. for 16 h. After cooling to RT, 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 (0.301 g, 79%). LCMS (Method J): RT 2.29 min [M+H]+ 611.

1. waitat 90° C. for 16 h
2. temperatureAfter cooling to RT
3. customvolatiles were removed in vacuo
4. customthe resulting residue purified by column chromatography (Si—PCC, gradient 2-8% 2M NH3/MeOH in DCM)