Dimethylformamide → Methacrylic acid 1-chlorocarbonyl-1,1-difluoro-2-butyl ester

Participants

Reaction Conditions

Reaction Steps

Into a 3-L vessel with a dropping funnel, added were 420 g (purity 56%, 1.25 mol) of methacrylic acid 1-hydroxycarbonyl-1,1-difluoro-2-butyl ester obtained in Example 1-3 and 7.50 g (0.11 mol/0.01 eq) of dimethylformamide. Then, 452 g (3.79 mol/0.01 eq) of thienyl chloride were dropped into the vessel at room temperature. The resulting solution was heated to 75° C. and stirred for 4 hours. The completion of the reaction was confirmed by 19F NMR. After that, the solution was distillated under a reduced pressure. With this, 255 g of methacrylic acid 1-chlorocarbonyl-1,1-difluoro-2-butyl ester was obtained (yield: 92%, purity: 98%).

Provenance & Evidence