反应详情

温度

50 °C

In THF (10 ml) was dissolved 5-dimethylamino-4-formyl-2-methyl-3(2H)-pyridazinone (362 mg) followed by dropwise addition of 3.0M methylmagnesium bromide/diethyl ether (1.0 ml) with ice-cooling, and the mixture was stirred at 50° C. for 30 minutes. To this reaction mixtrue was added 1N-hydrochloric acid (3 ml) with ice-cooling. Then, saturated aqueous NaHCO3 solution was added and the mixture was extracted with ethyl acetate. The organic layer was washed with saturated aqueous NaCl solution, dried over anhydrous magnesium sulfate, and concentrated to dryness. Yellow oil, 371 mg. 1H-NMR (CDCl3) δ: 1.64(3H,d,J=6.6Hz), 2.94(6H,s), 3.72(3H,s), 4.93(1H,dq,J=6.6&11.4Hz), 5.31(1H,d,J=11.4Hz), 7.66(1H,s).

1. temperaturecooling
2. temperaturecooling
3. extractionthe mixture was extracted with ethyl acetate
4. washThe organic layer was washed with saturated aqueous NaCl solution
5. dry with materialdried over anhydrous magnesium sulfate
6. concentrationconcentrated to dryness