Preparation method of propionic acid clobetasol
A technology of clobetasol propionate and a manufacturing method, which is applied in the manufacturing field of clobetasol propionate, can solve problems such as environmental pollution, unsafe production and operation, achieves high yield, low risk and hazard, The effect of simple reaction steps
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Embodiment 1
[0024] First, 13 kg of betamethasone 17-propionate sulfonate was mixed with 20 kg of anhydrous lithium chloride, dissolved in 100 kg of dimethylformamide (DMF), while the stirring speed was 100 rpm, and the mixing temperature was 95°C. The reaction time is 3 hours for chlorination reaction; second, after the chlorination reaction is complete, water analysis is carried out through 600 kg of ice water at a temperature of 10°C for 1 hour; 4000rpm, time 30 minutes, then at a temperature of 75 ° C, time 5 hours to dry after 11 kg of clobetasol propionate crude product; third, then dissolve the clobetasol propionate crude product in 150 kg of ethanol, and add 3 kg of activated carbon, decolorization, filtration, decolorization and filtration refers to heating temperature 50 ℃, time 1 hour, stirring speed 70rpm, stirring time 1 hour conditions, recovery of activated carbon; fourth, the filtrate is vacuum degree -0.08MPa, temperature 50 ℃, time 30 minutes, stirring speed 80rpm, stirri...
Embodiment 2
[0026] First, 13 kg of betamethasone 17-propionate sulfonate was mixed with 15 kg of anhydrous lithium chloride, dissolved in 100 kg of dimethylformamide (DMF), while the stirring speed was 100 rpm, and the mixing temperature was 90°C. The reaction time is 3 hours for chlorination reaction; second, after the chlorination reaction is complete, water analysis is carried out through 550 kg of ice water at a temperature of 8°C for 1 hour; 4000rpm, time 30 minutes, and then at a temperature of 80 ° C, after drying for 5 hours, 11 kg of clobetasol propionate crude product was obtained; thirdly, the clobetasol propionate crude product was dissolved in 140 kg of methanol, and added 3 kg of activated carbon, decolorization, filtration, decolorization and filtration refers to heating temperature 50 ℃, time 1 hour, stirring speed 70rpm, stirring time 1 hour conditions, recovery of activated carbon; fourth, the filtrate is vacuum degree -0.05MPa, temperature 50 ℃, time 30 minutes, stirrin...
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