Preparation method of halometasone
The technology of halogenmetasone and compound is applied in the field of preparation of halogenmetasone, which can solve the problems of unstable raw materials and high cost of dichloroflumetasone, and achieve the effects of convenient post-processing, improved product purity, and avoidance of being oxidized.
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Embodiment 1
[0025] 1) Chlorine reaction
[0026] Add 30g of the compound of formula 1 and 1000ml of dioxane as a solvent in the there-necked flask, heat to 50°C to dissolve it, cool the reaction solution to 0-5°C under an ice bath, then dissolve 270ml of chlorine gas propionic acid solution (36g of chlorine gas in 500ml of propionic acid) was added dropwise into the reaction solution in three batches, and the reaction solution was reacted in the dark at 5-10°C for 3 days. After the reaction was completed, the reaction solution was poured into 1 liter of ice water, extracted three times with 500 ml of dichloromethane, the organic phase was washed with water, saturated sodium bicarbonate solution, and water in turn, dried and filtered over sodium sulfate, and spun at 30 to 35 ° C. Dry the solvent to obtain compound 2, filter and dry to obtain 43 g of the crude compound shown in formula 2 (this compound is unstable, no further purification is required, and it is directly fed to the next step...
Embodiment 2
[0032] 1) Chlorine reaction
[0033] Add 30g of formula 1 compound and solvent 1000ml tetrahydrofuran into the there-necked flask, heat to 50°C to dissolve it, cool the reaction solution to 0-5°C under ice bath, then dissolve 270ml of chlorine gas propionic acid solution (36g chlorine gas in 500ml propionic acid Middle) was added dropwise into the reaction solution in three batches, and the reaction solution was reacted for 3 days in the dark at 20-25°C. After the reaction was completed, the reaction solution was poured into 1 liter of ice water, extracted 3 times with 500ml of dichloromethane, the organic phase was washed with water, saturated sodium bicarbonate solution, and water in turn, dried and filtered over sodium sulfate, and spun at 30-35°C. The compound 2 obtained by drying the solvent was filtered and then dried to obtain 41 g of the crude compound shown in formula 2 (this compound is unstable, no further purification is required, and it is directly fed to the next...
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