A kind of preparation method of 3 chloromethyl oxycephem antibiotic mother nucleus
A technology of chloromethyloxycephem and antibiotics, which is applied in the field of drug synthesis, can solve the problems of unfavorable industrial production, cumbersome and lengthy steps, and unfriendly environment, and achieve the goal of improving optical purity and chemical purity, shortening the process route, and single product Effect
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Embodiment 1
[0032] 100g of intermediate 1 was dissolved in 800ml of tetrahydrofuran, 29g of N,N-diisopropylethylamine was added, and reacted at -45°C for 2h. After cooling to room temperature, 100ml of water was slowly added to quench the reaction. At room temperature, the system was poured into 100ml of ethyl acetate, and the layers were separated after standing. The organic phase was extracted once with 80ml of 10% by mass dilute hydrochloric acid solution, then once with 80ml of water, once with 80ml of saturated saline, and finally added with 10g of anhydrous sodium sulfate to dry for 10h. After suction filtration, the filtrate was evaporated to dryness under reduced pressure, and the residue was recrystallized with 5 ml of ethanol to obtain Intermediate 2. Yield 97%.
[0033] 10g of intermediate 2 was dissolved in 30ml of carbon tetrachloride, 3g of N-chlorosuccinimide and 2g of dibenzoyl peroxide were added, and the reaction was carried out under reflux for 6 hours. TLC detected t...
Embodiment 2
[0040] 100g of intermediate 1 was dissolved in 800ml of acetone, 29g of n-butyllithium was added, and reacted at 0°C for 2h. After cooling to room temperature, 100ml of water was slowly added to quench the reaction. At room temperature, the system was poured into 100ml of ethyl acetate, and the layers were separated after standing. The organic phase was extracted once with 80ml of 10% by mass dilute hydrochloric acid solution, then once with 80ml of water, once with 80ml of saturated saline, and finally added with 10g of anhydrous sodium sulfate to dry for 10h. After suction filtration, the filtrate was evaporated to dryness under reduced pressure, and the residue was recrystallized with 5 ml of ethanol to obtain Intermediate 2. Yield 96%.
[0041] 10 g of intermediate 2 was dissolved in 30 ml of dichloromethane, 3 g of N-chlorosuccinimide and 2 g of azobisisobutyronitrile were added, and the reaction was carried out under reflux for 6 h. TLC detected that the reaction was c...
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