反应详情

温度

130 °C

A mixture of 6-bromo-1-chlorophthalazine (Example 1, 90 mg, 370 μmol), 2-isopropyl-2,5-diaza-bicyclo[2.2.1]heptane dihydrochloride (95 mg, 444 μmol) and potassium carbonate (153 mg, 1109 μmol) in 10 mL acetonitrile was stirred at 130° C. under in a sealed tube. The mixture turned red in about 5 min. The reaction was monitored by MS. After about 1 h at 130° C., MS and TLC showed all starting material was converted to product (M+1=347, 349). The mixture was cooled down to room temperature, and concentrated on a Rotavaporator. After purification by column (eluting with gradient of 2-10% 2M ammonia in methanol to DCM), 2-(6-bromophthalazin-1-yl)-5-isopropyl-2,5-diaza-bicyclo[2.2.1]heptane (60 mg) was obtained as a yellow solid.

1. waitAfter about 1 h at 130° C.
2. temperatureThe mixture was cooled down to room temperature
3. concentrationconcentrated on a Rotavaporator
4. customAfter purification
5. washby column (eluting with gradient of 2-10% 2M ammonia in methanol to DCM)