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Preparation method of 2-benzo diazepine anthrone

A technology of dibenzoazepine and anthrone, which is applied in the field of preparation of dibenzoazepine, can solve the problems of low yield and many by-products, and achieve the effect of high yield and high purity of raw materials

Active Publication Date: 2013-06-05
XUZHOU B&C CHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

But its yield is relatively low, and by-products are more

Method used

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  • Preparation method of 2-benzo diazepine anthrone
  • Preparation method of 2-benzo diazepine anthrone
  • Preparation method of 2-benzo diazepine anthrone

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Embodiment Construction

[0018] Below in conjunction with embodiment, the present invention is described further.

[0019] 1. Overall reaction equation:

[0020]

[0021] 2. Overview of each step:

[0022] first step:

[0023] 1. Reaction equation:

[0024]

[0025] 2. Ratio of materials:

[0026]

[0027] 3. Operation steps:

[0028] Add 270g of anthrone, 500g of dichloromethane, 2430g of concentrated sulfuric acid into a 5000ml reaction bottle, mechanically stir, slowly add 126g of sodium azide at room temperature (it takes more than 12 hours, azido acid and nitrogen are generated, tail gas absorption, anti-virus), Then stir at room temperature for more than 10 hours. If the raw material does not react completely, continue to add sodium azide in batches until the raw material reacts completely (center control one). After the reaction of the raw materials is complete, slowly add the reaction solution into 5000g of ice water (note that a large amount of gas is generated, anti-virus), sti...

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Abstract

The invention discloses a preparation method of 2-benzo diazepine anthrone. The method comprises the following steps: anthranone, dichloromethane and concentrated sulfuric acid are filled in a reaction bulb according to a certain proportion, mechanical stirring is carried out, and sodium azide is slowly filled in the reaction bulb under room temperature to obtain yellow solid; the yellow solid and ammonia water are put in the reaction bulb to heat up to 80 DEG C to 90 DEG C, then zinc powder and copper sulfate are filled in batches, and the solution is stirred for 24 hours to 40 hours. Thin-layer chromatography (TLC) detection is carried out to confirm that no raw materials is left, the solution is cooled to room temperature, the zinc power is filtered out, and the zinc powder is washed for 3 to 4 times by ammonia water of 10%. PH is adjusted to 4 to 5 through acid under the room temperature, the solution is cooled to the temperature lower than 5 DEG C, and is stirred, and suction filtration is carried out, mother solution is extracted through ethyl acetate, organic phase is washed with Na2S solution, Na2SO4 is dried and concentrated, and crude products are obtained through filter cakes and the organic phase; and the crude products and toluene are put into the reaction bulb, and products are obtained after a series of reactions. The purity of the raw materials of the preparation method of the 2-benzo diazepine anthrone is high, and the yield coefficient of the obtained product is quite high.

Description

technical field [0001] The invention relates to the field of chemical industry, in particular to a preparation method of dibenzoazepine. Background technique [0002] Benzodiazepines are a class of benzo seven-membered heterocyclic compounds with important pharmacological and physiological activities, and are often used as drugs for the treatment of nervous system and cardiovascular system diseases. This kind of compound also has antifungal, antibacterial, antiviral and antagonistic effects, and has been widely used in medical treatment with good effects. Therefore, the research on its unique chemical structure and special physiological activity has been widely concerned by people. The results of the study found that the ester group and carboxyl group at different positions of the seven-membered ring of benzozapine are active groups, which can effectively increase its antibacterial activity. In order to study and discover heterogeneous compounds with high antibacterial acti...

Claims

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Application Information

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IPC IPC(8): C07D223/20
Inventor 贺宝元邵严亮刘聪夏民鑫宋宝发彭剑平
Owner XUZHOU B&C CHEM CO LTD
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