A kind of synthetic method of progesterone
A synthesis method and technology of progesterone are applied in the field of preparation technology of steroid hormone drugs, which can solve the problems of long synthesis route of progesterone, unavailable raw materials, high cost, etc., to facilitate industrial implementation, avoid the use of toxic and harmful reagents, The effect of improving the reaction yield
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Embodiment 1
[0036] The present embodiment provides a kind of synthetic method of progesterone, it may further comprise the steps:
[0037] (1) Elimination reaction
[0038] Add 20 g and 250 g of benzene of the compound of formula (II) into the reaction flask, stir and dissolve the material, add 2 g of boron trifluoride diethyl ether, heat up to 80° C. for reflux reaction, and reflux reaction for 4 hours. TLC (thin layer chromatography) detects no reaction. The raw material was cooled to 50°C, and 200ml of water was added to terminate the reaction, and the layers were washed until neutral. Concentrate benzene under reduced pressure to a paste, add 30 g of methanol to remove benzene, add 30 g of methanol, stir and crystallize, cool to 0-5 ° C, keep warm for 30 minutes, filter with suction, and dry at 70 ° C to constant weight to obtain light yellow formula (Ⅲ ) compound 18.4g, HPLC content 98.5%, yield 92.0%.
[0039] It can be seen that boron trifluoride diethyl ether is selected as the ...
Embodiment 2
[0045]The present embodiment provides a kind of synthetic method of progesterone, it may further comprise the steps:
[0046] (1) Elimination reaction
[0047] Add 20 g and 250 g of benzene of the compound of formula (II) into the reaction flask, stir and dissolve the materials, add 10 g of p-toluenesulfonic acid, heat up to 80° C. for reflux reaction, and reflux for 6 hours. TLC (thin layer chromatography) detects that there is no raw material in the reaction. , lower the temperature to 50°C, add 200ml of water to terminate the reaction, and wash the layers until neutral. Concentrate benzene under reduced pressure to a paste, add 30 g of methanol to remove benzene, add 30 g of methanol, stir and crystallize, cool to 0-5 ° C, keep warm for 30 minutes, filter with suction, and dry at 70 ° C to constant weight to obtain light yellow formula (Ⅲ ) Compound 18.0g, HPLC content 98.0%, yield 90.0%.
[0048] (2) oxidation reaction
[0049] Add 18.0g of the compound of formula (Ⅲ) a...
Embodiment 3
[0053] The present embodiment provides a kind of synthetic method of progesterone, it may further comprise the steps:
[0054] (1) Elimination reaction
[0055] Add 20g of the compound of formula (II) and 250g of dichloromethane into the reaction flask, stir and dissolve the materials, cool the system down to 0-5°C, add 20ml of concentrated sulfuric acid dropwise, and control the temperature at 0-5°C. React at ~5°C for 2 hours, TLC (thin layer chromatography) detects that there is no raw material in the reaction, add 200ml of water to terminate the reaction, and wash through layers until neutral. Concentrate the dichloromethane under reduced pressure, take up the dichloromethane with water, add 200 ml of water for water analysis, and filter to obtain 19.0 g of light yellow compound of formula (III), with a yield of 95.0%.
[0056] (2) oxidation reaction
[0057] Add 19.0g of the compound of formula (Ⅲ) and 200g of acetone into the reaction flask, stir and dissolve the materi...
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