One-pot method for preparing the method of benzoyl corilide
A technology of benzoylide and ketolide, applied in organic chemistry methods, organic chemistry and other directions, can solve the problems of many side reactions, difficult process conditions, large consumption of materials, etc., to improve product purity and save organic Solvent, the effect of speeding up the reaction
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[0050] (A) Preparation of Corylidene Diol Primary Hydroxyl Derivatives: Add Solvent S to a Reactor with Filter Element at the Bottom 1 , add corylactone diol, stir until dissolved, then add triphenylchloromethane to carry out the alkylation reaction at the primary hydroxyl position, stir and react at a temperature of 10-30°C for 6-12h, until the reaction is complete, to obtain Solvent S containing primary hydroxyl derivatives of corylidene diol 1 reaction system;
[0051] (B) preparation of the diol derivatives of corylidene diol: the solvent S obtained in the step (A) 1 Under the condition of controlling the temperature of the reaction system at 0-30°C, add benzoyl chloride dropwise to carry out the hydrolysis reaction at the position of the primary hydroxyl group, and stir the reaction for 1-6 hours until the reaction is complete; add pure water and stir for 1-3 hours, inject nitrogen into the reaction kettle, Press filter, add solvent S 2 , refluxed for 1-4 hours, cooled...
Embodiment 1
[0109] Embodiment 1: One-pot method prepares (+) benzoyl cori lactone
[0110] Add 5L of pyridine to the reactor with a filter element at the bottom, add (+) 1 kg (1 eq) of corylidene diol with stirring, add 1.62 kg (1 eq) of triphenylchloromethane, and control the temperature at 10°C for 24 hours until complete reaction , add 670ml (1eq) of benzoyl chloride dropwise, and react at a temperature of 20°C for 6h until complete reaction; add 10L of pure water to the reaction kettle and stir for 3h to obtain a suspension. Hydraulically filter, then add 5L of methanol to the reactor, heat and reflux for 2h, filter the liquid to obtain solid powder; add 10L of acetonitrile to the reactor, add 14L of 1mol / L hydrochloric acid aqueous solution dropwise, and react at 30°C for 12h until complete Reaction, the temperature of the reaction system was lowered to 20°C, and saturated aqueous sodium bicarbonate solution was added to neutralize the reaction until pH = 7; the solvent acetonitrile ...
Embodiment 2
[0111] Embodiment 2: One-pot method prepares (-) benzoyl cori lactone
[0112] Add 6L of pyridine to the reactor with a filter element at the bottom, add (-) corylactone diol 0.8kg (1eq) under stirring, add 1.55kg (1.2eq) triphenylchloromethane, and react at a temperature of 20°C for 10h to For complete reaction, add 590ml (1.1eq) of benzoyl chloride dropwise, and react at a temperature of 30°C for 3 hours until complete reaction; add 24L of pure water to the reaction kettle and stir for 1 hour to obtain a suspension. The filter element will be suspended and hydraulically filtered, then add 8L of ethanol to the reaction kettle, heat and reflux for 1h, filter the liquid to obtain solid powder; add 16L tetrahydrofuran to the reaction kettle, add 8L 3mol / L hydrochloric acid aqueous solution dropwise, and control the temperature at 45°C for reaction After 4 hours to complete the reaction, cool the reaction system to 10°C, add saturated aqueous sodium carbonate solution to neutrali...
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