反应详情

温度

160 °C

A mixture of 3-(1-chlorophthalazin-6-yl)-N-cyclopropyl-4-methylbenzamide (300 mg, 888 μmol), 4,5,6,7-tetrahydro-1H-pyrazolo[3,4-c]pyridin-3-ol (247 mg, 1776 μmol) and N,N-diisopropylethylamine (310 μl, 1776 μmol) in NMP (3 mL) was heated to 160° C. for 18 h. After cooling to RT, the mixture was diluted with H2O and extracted with 25% i-PrOH/CHCl3 (3×). The combined organics were dried over Na2SO4, filtered and concentrated. The residue was purified with reverse-phase chromatography (Phenomenex Synergi 4m Max RP 80 A column, 150×21 mM, 20 mL/min, 10-95% CH3CN/H2O, 0.1% TFA, 10.5 min gradient) to obtain the title compound. MS (ESI, pos. ion) m/z: 441 (M+1).

1. temperatureAfter cooling to RT
2. extractionextracted with 25% i-PrOH/CHCl3 (3×)
3. dry with materialThe combined organics were dried over Na2SO4
4. filtrationfiltered
5. concentrationconcentrated
6. customThe residue was purified with reverse-phase chromatography (Phenomenex Synergi 4m Max RP 80 A column, 150×21 mM, 20 mL/min, 10-95% CH3CN/H2O, 0.1% TFA, 10.5 min gradient)