Preparation method of ciclesonide
The technology of a ciclesonide and a synthesis method is applied in the field of preparation of a glucocorticoid-type asthma therapeutic drug ciclesonide, and can solve the problems of difficult separation of impurities, low yield, expensive raw materials for ciclesonide reaction, and the like, To achieve the effect of reducing production cost, high yield and beneficial to industrial production
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[0033] The invention discloses a preparation method of ciclesonide, and those skilled in the art can learn from the content of this paper and appropriately improve the process parameters to achieve. It should be specially pointed out that all similar substitutions and modifications are obvious to those skilled in the art, they are all considered to be included in the present invention, and relevant persons can obviously do so without departing from the content, spirit and scope of the present invention. The content described herein can be modified or appropriately changed and combined to realize and apply the technology of the present invention.
[0034] In the present invention, unless otherwise specified, scientific and technical terms used herein have the meanings commonly understood by those skilled in the art.
Embodiment 1
[0036] Example 1: Preparation of compound of formula II
[0037]
[0038]At the temperature of -5~5℃, 100mL methanol was used as the solvent, the reaction flask was placed in an ice-water bath to control the low temperature, 5.4g (17.5mmol) of compound I, 4.2g (105mmol) of sodium hydroxide were added to the reaction flask, and stirred for 10~ 30min, under the dark condition, add 8.5g (26.3mmol) iodobenzene diacetate at one time, naturally rise to room temperature and react for 6~8 hours, monitor the reaction progress by TLC, drip 20g (141mmol) iodomethane, continue the reaction, wait for After the reaction, the solvent was removed under reduced pressure, extracted with 100 mL of ethyl acetate and 20 mL of water, the organic phase was washed with water, dried over anhydrous sodium sulfate, and the solvent was removed under reduced pressure to obtain 6.3 g (16.3 mmol) of the compound of formula II with a yield of 93 %.
Embodiment 2
[0039] Example 2: Preparation of compound of formula III
[0040]
[0041] 150 mL of acetone was used as a solvent, 7.1 g (18.4 mmol) of the compound of formula II was added, the temperature was lowered to -5 to 5 °C, 2.8 mL of about 3.4 g (73.4 mmol) of formic acid was added as a catalyst, and 5.2 g (33.1 mmol) of potassium permanganate were added. Oxidation reaction, TLC monitoring reaction progress, after the reaction is completed, the excess potassium permanganate is treated with saturated sodium sulfite solution, the insoluble solid is removed by filtration, washed with acetone, decolorized with activated carbon, the solid is removed by filtration, the solvent is removed under reduced pressure, and the pure water is recrystallized to obtain formula III Compound 6.8 g (16.2 mmol), 88% yield.
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