反应详情

温度

75 °C

A 250 mL round bottom flask is charged with 6-methyl-4-(1-propyl-butyl)-pyridazin-3-ylamine (0.611 g, 0.00295 moles, 1 equiv), ethanol 2B (30 mL), and chloroacetone (0.382 g, 0.328 ml, 0.00412 moles, 1.4 equiv). The reaction mixture is heated at 75° C. overnight and then cooled to room temp. NaHCO3 (0.371 g, 0.00442 moles, 1.5 equiv) is slowly added to the reaction mixture that is then heated to 100° C. overnight. The reaction mixture is cooled and the solvent is evaporated. Dichloromethane is added and the reaction mixture is passed through filter paper. The solvent is evaporated to obtain a brown oil which is purified via silica gel chromatography. The material is eluted with a hexanes and ethyl acetate gradient to obtain 0.511 g of the final products. Two peaks are identified in the lc/ms. The mixture is used “as is” in the next reaction. MS (APCI): 246 (M+1).

1. temperaturecooled to room temp
2. temperatureis then heated to 100° C. overnight
3. temperatureThe reaction mixture is cooled
4. customthe solvent is evaporated
5. additionDichloromethane is added
6. filtrationthrough filter paper
7. customThe solvent is evaporated
8. customto obtain a brown oil which
9. customis purified via silica gel chromatography
10. washThe material is eluted with a hexanes and ethyl acetate gradient