Poly (epsilon-caprolactone) supported anti-tumor prodrug and preparation method thereof
An anti-tumor drug, anti-tumor technology, applied in the direction of anti-tumor drugs, pharmaceutical formulations, medical preparations with inactive ingredients, etc. High rate, wide application, low cost effect
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[0066] 1. Preparation of α-position bromocyclohexanone
[0067] Add 20.00g (0.20mol) cyclohexanone, 38.14g (0.21mol) N-bromosuccinimide, 1.54g (0.02mol) ammonium acetate and 300mL anhydrous ether into a 500mL bottom flask equipped with a magnet, Clamp it on the iron frame platform, then install a condenser tube, connect a nitrogen bag to the condenser tube, and react at 25°C for 0.5h; after the reaction is completed, filter and wash the filtrate three times with distilled water; dry the organic phase with anhydrous magnesium sulfate , filtered, and after concentrating the solvent, separated on a silica gel column (petroleum ether / ethyl acetate=10:1) to obtain 30.09 g (85.0%) of a light yellow oily liquid.
[0068] 2. Preparation of α-brominated ε-caprolactone
[0069] Add 17.70g (0.10mol) α-position bromocyclohexanone and 20.64g (0.12mol) m-chloroperoxybenzoic acid to a 500mL single-necked round bottom flask equipped with a magnet, then add 300mL dichloromethane, at 25°C Und...
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