methyl 3-(1H-pyrazol-1-yl)propanoate synthesis

Yield:89943-28-2 98%

Reaction Conditions:

with Cs₂CO₃ in 1,4-dioxane at 105 - 115; for 6 h;Schlenk technique;

Steps:

22 A process for the preparation of a pyrazole derivative

(1) 1.5 mmol of methyl acrylate (129.1 mg, 1.5 mmol), 2.25 mmol of pyrazole (153.2 mg,), 5 mol% cesium carbonate (24.4 mg, 0.075 mmol, 5 mol%) and 5 mL of 1, 4-Dioxane were successively added to a dry Schlenk reaction tube with a cold finger and stirred at a reflux temperature of 105 to 115 ° CThe reaction mixture was stirred for 6 hours until the reaction was complete by TLC.(2) Add 10 mL of ethyl acetate to the reaction mixture and extract at room temperature to obtain the organic phase.The organic phase was washed successively with 5 mL of water, 5 mL of saturated brine, dried over anhydrous Na2SO4,And concentrated under reduced pressure to remove the solvent to give the crude product.The crude product was subjected to silica gel column chromatography to obtain 226.6 mg

References:

CN104030984,2016,B Location in patent:Paragraph 0194-0199