Preparation method for 1-fluoro-1,3-propane sultone
A technology of propane sultone and propene sultone is applied in the field of compound preparation to achieve the effects of ensuring superior performance, improving battery voltage and high yield
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Embodiment 1
[0025] Using dichloromethane as a solvent and benzoyl peroxide as a catalyst, add 1mol of 1,3-propene sultone to 200ml of dichloromethane, then introduce 1mol of HBr gas into it, and then add The catalyst is benzoyl peroxide, the reaction temperature is controlled at 10° C., and the reaction time is 1 h to obtain 1-bromo-1,3-propane sultone, which is rectified and the calculated yield is 46%.
[0026] Add 200 g of the above-prepared 1-bromo-1,3-propane sultone into 200 ml of sulfolane for dissolution, add 42 g of NaF and carry out F exchange reaction at 20°C for 2 hours to obtain 1-fluoro-1,3-propane sulfonate Acid lactone, the calculated yield is 46%, the purity is 99.5%, and the product moisture is 19PPM.
Embodiment 2
[0028] With dichloromethane as a solvent and benzoyl peroxide as a catalyst, 1mol of 1,3-propene sultone was added to 400ml of dichloromethane, and then 1.5mol of HBr gas was passed into it, and then The catalyst benzoyl peroxide was added, the reaction temperature was controlled at 35° C., and the reaction time was 5 hours to obtain 1-bromo-1,3-propane sultone, which was rectified and the calculated yield was 74.4%.
[0029] Add 200 g of the above-prepared 1-bromo-1,3-propane sultone into 400 ml of sulfolane for dissolution, add 84 g of NaF and carry out F exchange reaction at 40°C for 5 hours to obtain 1-fluoro-1,3-propane sulfonate Acid lactone, the calculated yield is 55.4%, the purity is 99.7%, and the product moisture is 17PPM.
Embodiment 3
[0031] Using dichloromethane as a solvent and benzoyl peroxide as a catalyst, add 1mol of 1,3-propene sultone to 800ml of dichloromethane, then introduce 2mol of HBr gas into it, and then add The catalyst is benzoyl peroxide, the reaction temperature is controlled at 50° C., and the reaction time is 10 h to obtain 1-bromo-1,3-propane sultone, which is rectified and the calculated yield is 87.2%.
[0032] Add 200 g of the above-prepared 1-bromo-1,3-propane sultone into 800 ml of sulfolane for dissolution, add 116 g of KF and carry out F exchange reaction at 60°C for 10 hours to obtain 1-fluoro-1,3-propane sulfonate Acid lactone, the calculated yield is 65.6%, the purity is 99.9%, and the product moisture is 16PPM.
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