Preparation method of isoflurane
A technology of isoflurane and freon, which is applied in the field of preparation of isoflurane, can solve the problems of low conversion rate, high cost and high risk, and achieve the effects of simple operation, avoiding chlorination process and simple reaction conditions
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Embodiment 1
[0035] Add 50% NaOH aqueous solution (160g) into the autoclave, close the autoclave, vacuumize, start stirring, add Freon-22 (87g), then feed nitrogen, control the temperature at 30-35°C, and stir for 2 hours. Difluoromethanol solution was obtained.
[0036] Feed Freon-123 (230g) into the above-mentioned high-pressure reaction kettle, and nitrogen gas was passed into after the addition was completed, and the reaction was stirred and reacted at 30-35°C for 3 hours. Phase, (3×30mL) washed with purified water to obtain isoflurane solution, and rectified to collect fractions at 48-49°C to obtain pure isoflurane with a yield of 88.3% (based on consumed Freon-22) and a purity of 99.88% .
Embodiment 2
[0038] Add 50% NaOH aqueous solution (144g) into the autoclave, close the autoclave, evacuate, start stirring, add Freon-22 (87g), then feed nitrogen, control the temperature at 30-35°C, and stir for 2.5 hours. Difluoromethanol solution was obtained.
[0039] Feed Freon-123 (230g) into the above-mentioned high-pressure reaction kettle, and nitrogen gas was passed into after the addition was completed, and the reaction was stirred and reacted at 20-25°C for 3.5 hours. Phase, (3×30mL) washed with purified water to obtain isoflurane solution, and rectified to collect fractions at 48-49°C to obtain pure isoflurane with a yield of 86.3% (based on consumed Freon-22) and a purity of 99.85% .
Embodiment 3
[0041] Add 50% NaOH ethanol solution (136g) into the autoclave, close the autoclave, vacuumize, start stirring, add Freon-22 (87g), then pass in nitrogen, control the temperature at 30-35°C, and stir for 3 hours , to difluoromethanol solution.
[0042] Feed Freon-123 (230g) into the above-mentioned high-pressure reaction kettle, and nitrogen gas was passed into after the addition was completed, and the reaction was stirred and reacted at 15-20°C for 3 hours. The lower organic phase was washed with (3×30mL) purified water to obtain isoflurane solution, and the fraction at 48-49°C was collected by rectification to obtain pure isoflurane with a yield of 84.8% (based on consumed Freon-22), purity 99.66%.
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