Synthetic method of cabazitaxel
A cabazitaxel and synthetic method technology, which is applied in the production of bulk chemicals, organic chemistry and other directions, can solve the problems of the general Raney nickel reduction yield, the high cost of cabazitaxel, and the waste of materials, and achieves low price and high yield. The effect of improving the efficiency and reducing the production cost
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Embodiment 1
[0054] route 1
[0055] (1) formula II-1 Compound Synthesis:
[0056] In a 250ml three-neck flask, under nitrogen protection, dissolve 10.81g of 10-deacetylbaccatin III in 100ml of anhydrous pyridine, cool down to 0°C and stir for 10 minutes, dissolve 8ml of trichloroethyl chloroformate in 50ml of anhydrous In dichloromethane, slowly drop into the reaction solution, keep stirring at 0°C for 30 minutes, rise to room temperature and stir for 30 minutes, slowly add a small amount of water dropwise to terminate the reaction, concentrate the reaction solution to oil, add 100ml of dichloromethane to dissolve, Wash with 2M hydrochloric acid until the water layer is acidic, then wash with saturated sodium bicarbonate solution (50ml×2), water (50ml×2), saturated sodium chloride solution (50ml×2), stir, and wash with anhydrous Dry over magnesium sulfate for 2 hours, filter, and spin dry. Add 20ml of diethyl ether / petroleum ether (volume ratio 1 / 1) mixed solution, stir at room tem...
Embodiment 2
[0075] route 2
[0076] (1) Synthesis of formula II-2 compound 7,10-bis(trichloroethoxycarbonyl)-10-deacetylbaccatin III:
[0077] Referring to the method described in Example 1, the compound of formula II-2 was obtained with a yield of 91.2%.
[0078] (2) Synthesis of the compound of formula III-2:
[0079] Dissolve 3.44g of 7,10-bis(trichloroethoxycarbonyl)-10-deacetylbaccatin III in 50ml of pyridine, then slowly drop into 0.62g of TESCl (triethylchlorosilane) and heat to 120 ℃, stirred for 4 hours, added 100ml of water to the reaction solution, then extracted the aqueous layer with ethyl acetate (100ml×3), combined the organic layers, washed with water (50ml×2), washed with saturated brine (50ml×2), added Dry over magnesium sulfate, and use petroleum ether / dichloromethane (volume ratio 2 / 1) silica gel column chromatography to obtain 2.92g of 7,10-bis(trichloroethoxycarbonyl)-13-triethylchlorosilane- 10-Deacetylbaccatin III, yield 90.0%.
[0080] 1 H-NMR (400 MHz, CD...
Embodiment 3
[0094] route 3
[0095] (1) Synthesis of the compound of formula II-3:
[0096] In a 250ml three-neck flask, under nitrogen protection, dissolve 10.81g of 10-deacetylbaccatin III in 100ml of anhydrous pyridine, cool down to 0°C and stir for 10 minutes, dissolve 8ml of methoxyethoxymethane in 50ml of anhydrous di In methyl chloride, slowly add the reaction solution dropwise, keep stirring at 0°C for 30 minutes, rise to room temperature and stir for 40 minutes, slowly add a small amount of water dropwise to terminate the reaction, concentrate the reaction solution to an oily state, add 100ml of dichloromethane to dissolve, and use Wash with 2M hydrochloric acid until the water layer is acidic, then wash with saturated sodium bicarbonate solution (50ml×2), wash with water (50ml×2), and saturated sodium chloride solution (50ml×2). Magnesium was dried for 2 hours, filtered and spin-dried. Add 20ml of diethyl ether / petroleum ether (volume ratio 1 / 1) mixed solution, stir at room...
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