Hydrochloric Acid → HCID 66860208, compound

Participants

Reaction Steps

5-Ethyl-2-hydrazinopyrimidine (400 mg, 2.89 mmol) was suspended in 3 mL of water, and acetylacetone (314 μL, 3.04 mmol) and 2 mol/L hydrochloric acid (330 μL) were added thereto and stirred at room temperature for 23 hours. 2 mL of sodium hydroxide aqueous solution was added to the reaction mixture to adjust the pH to 12. The mixture was extracted with ethyl acetate three times, and the organic phase was washed with saturated brine, dried over anhydrous sodium sulfate, and then filtrated. The filtrate was concentrated under reduced pressure, and the residue was purified by silica gel column chromatography (hexane:ethyl acetate=90:10→10:90) and silica gel column chromatography (methylene chloride:methanol=100:0→95:5) to give 203 mg of the title compound (yield 35%).

Provenance & Evidence