反应详情

温度

110 °C

A mixture of 6-(4-bromo-3-fluorophenyl)-1,2,4-triazin-3-amine (800 mg, 2.97 mmol) and 2-chloro-3-quinolin-6-ylpropanal (784 mg, 3.57 mmol) in isopropyl alcohol (10.0 mL) in a sealed tube was heated at 110° C. for 48 h. After the reaction mixture was cooled to ambient temperature, the product was precipitated and collected by filtration. The mother liquor was concentrated and the residue was dissolved in ethyl acetate, washed with aqueous sodium bicarbonate, water, brine, dried over magnesium sulfate, and concentrated under reduced pressure. The residue was purified on a silica gel column with methanol in dichloromethane (0-6%) to give the desired product. (65%) LCMS: (M+H)=434.0/436.0.

1. temperatureAfter the reaction mixture was cooled to ambient temperature
2. customthe product was precipitated
3. filtrationcollected by filtration
4. concentrationThe mother liquor was concentrated
5. dissolutionthe residue was dissolved in ethyl acetate
6. washwashed with aqueous sodium bicarbonate, water, brine
7. dry with materialdried over magnesium sulfate
8. concentrationconcentrated under reduced pressure
9. customThe residue was purified on a silica gel column with methanol in dichloromethane (0-6%)