反应详情

Acetyl chloride (41 g, 0.530 mol) was added dropwise to a solution of 3-methyl-1H-pyrazol-5-amine (25.6 g, 0.264 mol) and N-methylmorpholine (58 mL, 0.530 mol) in CH2Cl2 (250 mL) at 0° C. under an atmosphere of nitrogen. The reaction mixture was stirred at room temperature for 16 h. Water was added to the reaction mixture and the organic layer concentrated in vacuo. The residue was taken up in a mixture of MeOH/THF (100 mL/100 mL), cooled to 10° C. and treated with 1M NaOH solution. The reaction mixture was stirred for 0.25 h, acidified to pH 5 and organic solvents were removed in vacuo. The resulting precipitate was filtered, washed (water, diethyl ether) and dried to provide the title compound as a white solid (29.6 g).

1. concentrationthe organic layer concentrated in vacuo
2. additionThe residue was taken up in a mixture of MeOH/THF (100 mL/100 mL)
3. temperaturecooled to 10° C.
4. additiontreated with 1M NaOH solution
5. stirringThe reaction mixture was stirred for 0.25 h
6. customwere removed in vacuo
7. filtrationThe resulting precipitate was filtered
8. washwashed (water, diethyl ether)
9. customdried