反应详情

Acetic anhydride (12.7 mL, 134.8 mmol) was added dropwise to a solution of ethyl 2-(5-amino-3-phenyl-pyrazol-1-yl)acetate (31.5 g, 128.4 mmol) in pyridine (200 mL) at 0° C. under an atmosphere of nitrogen. Upon complete addition, the reaction mixture was warmed to room temperature and stirred for 16 h. The reaction mixture was concentrated in vacuo. The residue was diluted in CH2Cl2 (250 mL). The organic phase was washed with water and brine, dried (MgSO4), filtered and concentrated in vacuo. The residue was triturated from diethyl ether, filtered and dried to provide the title compound as a white solid (34.81 g).

1. additionUpon complete addition
2. concentrationThe reaction mixture was concentrated in vacuo
3. additionThe residue was diluted in CH2Cl2 (250 mL)
4. washThe organic phase was washed with water and brine
5. dry with materialdried (MgSO4)
6. filtrationfiltered
7. concentrationconcentrated in vacuo
8. customThe residue was triturated from diethyl ether
9. filtrationfiltered
10. customdried