Synthetic method of oxcarbazepine
A synthetic method, iminodibenzyl technology, applied in the field of synthesis of oxcarbazepine and oxcarbazepine (OCBZ), which can solve the problems of high price of starting materials, difficulty in obtaining starting materials, long process route, etc., and achieve Effects of low cost, simplified operation, and shortened synthesis process
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Embodiment 1
[0023] A synthetic method for oxcarbazepine, comprising the steps of:
[0024] 1) Preparation of iminodibenzoyl chloride by formyl chloride:
[0025] Add 50g (0.256mol) of iminodibenzyl and 250g of chlorobenzene into the reaction bottle, and slowly pass in 30.1g (0.307mol) of phosgene after heating up to 100°C, and absorb the tail gas with sodium hydroxide solution, and then Raise the temperature to 110-115°C and keep it warm for 4 hours to obtain a chlorobenzene solution of iminodibenzoyl chloride. Evaporate about 200 g of chlorobenzene under reduced pressure, cool down to room temperature, and precipitate a light green solid. Filter and dry to obtain iminodibenzoyl chloride. The light green solid of benzoyl chloride is about 53g, and the yield is 80%. The chlorobenzene mother liquor can be applied mechanically, and the yield can reach 99~100% after applying the mother liquor.
[0026] 2) Preparation of 10-bromo-5H-dibenzazepine-5-carbonyl chloride by double halo dehydrohal...
Embodiment 2
[0033] A synthetic method for oxcarbazepine, comprising the steps of:
[0034] 1) Preparation of iminodibenzoyl chloride by formyl chloride: same as Example 1;
[0035] 2) Preparation of 10-bromo-5H-dibenzazepine-5-carbonyl chloride by double halo dehydrohalogenation:
[0036] Add 62.2g (0.256mol) of iminodibenzoylchloride and 250g of chlorobenzene into the reaction flask, raise the temperature to 80°C, add 0.5g of azoisobutyronitrile, slowly add liquid bromine 94.1g (1.178mol), drop The acceleration is based on the bromine not escaping from the return pipe, and the tail gas is absorbed with sodium hydroxide solution. After the dropwise addition, keep warm for 2 hours, add 0.2g of azoisobutyronitrile, heat up and reflux, and then add 0.2g every 4 hours , added a total of 3 times, after the reaction was completed, the chlorobenzene was evaporated and then lowered to room temperature to obtain 10-bromo-5 H -dibenzazepine-5-formyl chloride crude product, directly carry out next...
Embodiment 3
[0040] A synthetic method for oxcarbazepine, comprising the steps of:
[0041] 1) Preparation of iminodibenzoyl chloride by formyl chloride:
[0042] Add 50g (0.256mol) of iminodibenzyl, 250g of chlorobenzene, and 30.1g (0.103mol) of triphosgene into the reaction bottle, slowly heat to 100°C, and absorb the tail gas with sodium hydroxide solution, and then lower the temperature after 30 minutes. Rise to 110~115°C and keep it warm for 4 hours, then cool down to room temperature to obtain a chlorobenzene solution of iminodibenzoyl chloride, and proceed directly to the next reaction.
[0043] 2) Preparation of 10-bromo-5H-dibenzazepine-5-carbonyl chloride by double halo dehydrohalogenation:
[0044] Add 84.1 g (0.295 mol) of dibromohydantoin and 0.5 g of benzoyl peroxide to the iminodibenzoyl reaction solution obtained in step 1), slowly add to 80 ° C, and use sodium hydroxide solution for the tail gas Absorption, 0.2 g of benzoyl peroxide was added after the heat preservation ...
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