2-CHLORO-N-(1,5-DIMETHYL-3-OXO-2-PHENYL-2,3-DIHYDRO-1H-PYRAZOL-4-YL)ACETAMIDE synthesis

Yield:3608-86-4 62%

Reaction Conditions:

with triethylamine in dichloromethane at 20;

Steps:

1.6 6.Preparation of 2-chloro-N- (1,5-dimethyl-3-oxo-2-phenyl-2,3-dihydro-1H-pyrazol-4-yl) acetamide (8)

Chloroacetyl chloride (9.04 g, 80 mmol) and triethylamine (8.08 g, 80 mmol) were added to 150 mL containing4-aminoantipyrine (16.24 g, 80 mmol) in DCM solution,Stir overnight at room temperature.Then add a certain volume of ice water to the solution for extraction, take the organic layer,The organic layer was first washed with a 1N HCl solution (3 × 100 mL),It was then washed with a saturated aqueous NaHCO3 solution (100 mL).It was then washed with brine (100 mL).After drying over MgSO4, the solvent was removed,25.15 g of a green solid are obtained.The crude product was recrystallized from DCM / MTBE,This gave 13.83 g of a white solid. The yield was 62%.

References:

CN110627774,2019,A Location in patent:Paragraph 0030; 0039; 0040