Method for preparing iminodibenzyl

A technology of adding phosphoric acid to iminodibenzyl and diaminobibenzyl, which is applied in the field of preparation of pharmaceutical intermediates, can solve the problems of difficult further improvement of product quality and complicated post-treatment process, and achieve good crystal form, high product yield and high product quality. The effect of high purity
CN102391182AActive Publication Date: 2012-03-28JIANGSU TOHOPE PHARMA
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Patent Information

Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
JIANGSU TOHOPE PHARMA
Publication Date
2012-03-28

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Abstract

The invention discloses a method for preparing iminodibenzyl. In the method, phosphoric acid is added into 2,2,-diamido-bibenzyl to form salt, and the salt is subjected to cyclization reaction to prepare the iminodibenzyl. The method is characterized in that after the phosphoric acid is separated from a product formed by the cyclization reaction of the 2,2,-diamido-bibenzyl, nitrogen is introduced to perform reduced pressure distillation, and the distilled iminodibenzyl is collected by a cyclone separator. The method for preparing the iminodibenzyl comprises the following steps of: adding the phosphoric acid into the 2,2,-diamido-bibenzyl to form the salt, performing the cyclization reaction to obtain iminodibenzyl, introducing the nitrogen directly, distilling under reduced pressure, and collecting the iminodibenzyl by the cyclone separator, wherein the product formed by the cyclization reaction is subjected to the steps of elutriation, recrystallization and the like. The method has a simple process, the yield of the product is improved, and the purity of the iminodibenzyl is over 99.0 percent.
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Description

technical field

[0001] The invention relates to a preparation method of a pharmaceutical intermediate, in particular to a preparation method of iminodibenzyl. Background technique

[0002] Iminodibenzyl, chemical name 10,11-dihydro-5H-dibenzo[b,f]azepine, is an important pharmaceutical intermediate and is used in the synthesis of carbamazepine, oxcarbazepine and promethazine hydrochloride Azine (structure shown in the following formula)

[0003]

[0004] It is the key intermediate of synthetic lubricating oil and important raw material of high temperature antioxidant. At present, the annual demand for iminodibenzyl in the global market has reached thousands of tons, and it is of great significance to explore and improve the production process of iminodibenzyl.

[0005] The preparation of iminodibenzyl is obtained by using o-nitrotoluene as the starting material through condensation, reduction and ring closure. The synthesis process used earlier in industrialized produc...

Claims

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