Preparation method of estra-4-ene-3,17-dione
A technology of estrogen and dione, which is applied in the preparation of estrogen-4-ene-3,17-dione and the chemical synthesis of steroid hormone drugs, which can solve the problems of high raw material cost, large environmental pollution, and long route , to achieve the effect of short synthetic route, low production cost and simple operation
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[0024] refer to figure 1 , which shows a flow chart of a preparation method of estro-4ene-3,17-dione described in the embodiment of the present invention, the method comprising the following steps:
[0025] Step 1, hydrogenation reaction: under the protection of nitrogen, add the first solvent and palladium catalyst to the reaction vessel, stir for 10-60min, pass hydrogen into the reaction vessel to replace the nitrogen, after the nitrogen replacement, add the first solvent to the reaction vessel Add the raw material with the general formula I into the container and stir, raise the temperature to 10-60° C., feed hydrogen gas for 2-10 hours, and filter out the palladium catalyst with nitrogen pressure after the reaction to obtain an intermediate solution of the compound with the general formula II. Reserve under nitrogen protection.
[0026] Preferably, during the hydrogenation reaction, the volume ratio of the mass of the raw material to the first solvent is 1:1-1:10.
[002...
Embodiment 1
[0040] (1) Hydrogenation reaction.
[0041] At room temperature, under the protection of nitrogen, add 200ml of ethanol to a 250ml clean and dry four-neck flask, stir, add 5g of palladium carbon, and stir for 30min. Hydrogen gas was used to replace nitrogen gas. After passing hydrogen gas for 30 minutes, 20 g of raw material was added, the temperature was raised to 50° C., hydrogen gas was passed for 6 hours, and the reaction was detected by HPLC. Palladium carbon was filtered out using nitrogen pressure to obtain an intermediate solution of the compound of general formula II, which was set aside under the protection of nitrogen.
[0042] (2) Ring closing reaction.
[0043] Under the protection of nitrogen, the intermediate solution of the compound having the general formula II was concentrated under normal pressure until it became viscous, 30 g of phosphoric acid was added, and the reaction was carried out at 80° C. for 3 h, and the reaction was completed by HPLC detection. ...
Embodiment 2
[0045] (1) Hydrogenation reaction.
[0046] At room temperature, under the protection of nitrogen, add 20ml of methanol to a 250ml clean and dry four-neck flask, stir, add 2g of palladium barium sulfate, and stir for 10min. Hydrogen gas was used to replace nitrogen gas. After 10 minutes of hydrogen gas flow, 20 g of raw material was added, the temperature was raised to 10° C., hydrogen gas was passed for 2 h, and the reaction was detected by HPLC. The palladium barium sulfate was filtered out using nitrogen pressure to obtain an intermediate solution of the compound of general formula II, which was set aside under the protection of nitrogen.
[0047] (2) Ring closing reaction.
[0048] Under the protection of nitrogen, the intermediate solution of the compound with general formula II was concentrated under normal pressure until it became viscous, 10 g of perchloric acid was added, and the reaction was carried out at 60° C. for 5 h, and the reaction was completed by HPLC detec...
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