Taxane compound and preparation method thereof
A compound and silane-based technology, applied in the preparation of intermediate compounds of cabazitaxel, in the field of preparation of cabazitaxel, can solve problems such as low yield and increased synthesis cost of cabazitaxel
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example 1
[0139] Example 1: Preparation of Compound 1
[0140] (1) Preparation of Compound 3
[0141]
[0142] N 2 Under protection, 10-DAB (10.01g, 18.4mMol) was dissolved in 490ml DMF, and imidazole (4.99g, 73.3mMol) was added thereto, cooled to 0°C in an ice bath, and Et 3 SiCl (11.10g, 73.6mMol), after dropping, the temperature was maintained at 0°C for reaction, and TLC detected that the raw material disappeared after 2 hours.
[0143]Add 100ml of methyl tert-butyl ether and 200ml of water to the system successively, keep the temperature at about 0°C, stir for 15 minutes, separate the organic phase, continue to extract the water phase with methyl tert-butyl ether twice, combine the organic phases, The organic phase was washed twice with water and saturated brine, dried over anhydrous magnesium sulfate, and concentrated under reduced pressure to obtain a light yellow solid.
[0144] The resulting crude product was dissolved in 60 ml of dichloromethane, cooled and crystallized,...
example 2
[0164] The preparation of example 2 cabazitaxel
[0165] (1) Preparation of compound 6
[0166]
[0167] N 2 Under protection, compound 1 (5.00g, 4.75mMol) was dissolved in 50ml DCM, and Et was added dropwise thereto at 0°C 3 N.3HF (55.00ml, 341.91mMol), after dropping, the temperature gradually rose to 20°C. After stirring for 2.5 hours, TLC detected that the raw material disappeared, and the reaction solution was added dropwise to 1L saturated NaHCO 3 solution, after stirring for 30min, the organic phase was separated, the aqueous phase was extracted twice with 100ml DCM, and the organic phase was combined; the organic phase was washed twice with water and saturated brine successively, dried over anhydrous sodium sulfate, and the solvent was removed under reduced pressure to obtain 4.65g white solid.
[0168] The resulting crude product was recrystallized from dichloromethane / n-hexane (1 / 4, V / V) to obtain 4.26 g of compound 6 as a white solid, with a yield of 95.55%. ...
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