反应详情

温度

150 °C

A mixture of 12-chloro-4-[1-(propan-2-yl)-1H-1,2,4-triazol-5-yl]-9-oxa-3,6,13-triazatricyclo[8.4.0.02,6]tetradeca-1(14),2,4,10,12-pentaene (150 mg, 0.450 mmol), TEA (0.5 mL), and 4-(pyrrolidin-2-yl)pyridine (134 mg, 0.900 mmol) in NMP (0.5 mL) was stirred at 150° C. for 24 h under nitrogen atmosphere. The resulting mixture was purified by reverse phase combiflash eluting with a 0-50% gradient of CH3CN in 0.3% NH4HCO3 to give 136, which was further purified by chiral HPLC (AD column, 30% EtOH (0.1% DEA) in n-Hexane isocratic) to separate the (R) and (S) enantiomers, 23 mg of one enantiomer and 28 mg of the other (26% total yield).

1. customThe resulting mixture was purified by reverse phase combiflash
2. washeluting with a 0-50% gradient of CH3CN in 0.3% NH4HCO3