反应详情

温度

100 °C

A mixture of 2,2-dimethylpropionic acid 2-{(R)-3-[2-((S)-2-aminobutyrylamino)-5-fluorophenylamino]piperidin-1-yl}ethyl ester (0.588 g, 1.39 mmol), 6-chloro-9-(tetrahydropyran-2-yl)-9H-purine (0.333 g, 1.39 mmol), and DIPEA (0.71 mL, 4.15 mmol) in n-butanol (6 mL) was stirred in a sealed vial at 100° C. for 16 h. After cooling to RT, volatiles were removed in vacuo and the resulting residue purified by column chromatography (Si—PCC, gradient 2-10% 2M NH3/MeOH in DCM) affording the title compound as a light brown gum (0.516 g, 59%). LCMS (Method B): RT 2.47 min [M+H]+ 625.

1. temperatureAfter cooling to RT
2. customvolatiles were removed in vacuo
3. customthe resulting residue purified by column chromatography (Si—PCC, gradient 2-10% 2M NH3/MeOH in DCM)