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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

Active Publication Date: 2012-03-28
JIANGSU TOHOPE PHARMA
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0010] In the above method, post-treatment processes such as product separation and purification are complicated, and the product quality is difficult to further improve
In the open literature about the preparation method of iminodibenzyl, there are few reports about product separation and purification methods after cyclization

Method used

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  • Method for preparing iminodibenzyl
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  • Method for preparing iminodibenzyl

Examples

Experimental program
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Effect test

Embodiment 1

[0045] refer to figure 1 , figure 2 Shown technological process and equipment, prepare iminodibenzyl according to the method of the present invention.

[0046] Take 135kg2,2 ， - Diaminobibenzyl is heated to 260°C in a 300L reaction kettle, and 135 kg of industrial phosphoric acid (85% mass fraction) is added dropwise for one hour, then the temperature is raised to 260°C to 300°C, and the temperature is kept for 1 hour. After the reaction is completed, the phosphoric acid waste solution is divided.

[0047] Turn on the vacuum, introduce industrial nitrogen (nitrogen flow rate at 80L / min), and carry out vacuum distillation, that is, iminodibenzyl powder will be evaporated. The vacuum degree of the whole system is -0.080MPa, and the liquid phase temperature in the reactor is kept at 200 ℃~240℃. The powdery product is collected by a cyclone separator and settles at the bottom of the collection tank. The distillation time was 2 hours, and when there was no obvious material to...

Embodiment 2

[0050] Take 135kg2,2 ， - Diaminobibenzyl is heated to 260°C in a 300L reaction kettle, and 135 kg of industrial phosphoric acid (85% mass fraction) is added dropwise for one hour, then the temperature is raised to 260°C to 300°C, and the temperature is kept for 1 hour. After the reaction is completed, the phosphoric acid waste solution is divided.

[0051]Turn on the vacuum, introduce industrial nitrogen gas (nitrogen flow rate 120 L / min), and carry out vacuum distillation, that is, iminodibenzyl powder will be evaporated, and the vacuum degree of the whole system will be kept at -0.095 MPa, and the liquid phase temperature in the reactor will be kept at 200 ℃~240℃. The powdery product is collected by a cyclone separator and settles at the bottom of the collection tank. The distillation time was 1.5 hours. When the sight glass showed that there was no obvious material to evaporate, and the temperature of the gas phase dropped to 150°C, the distillation was stopped after exte...

Embodiment 3

[0053] Take 135kg2,2 ， - Diaminobibenzyl is heated to 260°C in a 300L reaction kettle, and 135 kg of industrial phosphoric acid (85% mass fraction) is added dropwise for one hour, then the temperature is raised to 260°C to 300°C, and the temperature is kept for 1 hour. After the reaction is completed, the phosphoric acid waste solution is divided.

[0054] Turn on the vacuum, introduce industrial nitrogen gas (nitrogen flow rate 100 L / min), and carry out vacuum distillation, that is, iminodibenzyl powder will be evaporated, and the vacuum degree of the whole system will be kept at -0.090 MPa, and the liquid phase temperature in the reactor will be kept at 200 ℃~240℃. The powdery product is collected by a cyclone separator and settles at the bottom of the collection tank. The distillation time was 1.5 hours. When the sight glass showed that there was no obvious material to evaporate, and the temperature of the gas phase dropped to 150°C, the distillation was stopped after ext...

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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.

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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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D223/22
Inventor 邹振荣
Owner JIANGSU TOHOPE PHARMA
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