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Refining method for 2,6-dichloro-4,8-dipiperidinopyrimidino[5,4-d]pyrimidine serving as dipyridamole intermediate

A technology of dipiperidium ion and purification method, applied in the direction of organic chemistry and the like, can solve the problems of many side reactions, extensive process, large impurity content of synthetic products, etc., and achieve the effects of less side reactions, better appearance and high yield.

Inactive Publication Date: 2015-12-16
芮城县虹桥药用中间体有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The current DDH synthesis process cannot meet the requirements of follow-up fine pharmaceuticals due to its extensive process, many side reactions, high impurity content in the synthetic product, and poor appearance and color of the product.

Method used

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  • Refining method for 2,6-dichloro-4,8-dipiperidinopyrimidino[5,4-d]pyrimidine serving as dipyridamole intermediate
  • Refining method for 2,6-dichloro-4,8-dipiperidinopyrimidino[5,4-d]pyrimidine serving as dipyridamole intermediate
  • Refining method for 2,6-dichloro-4,8-dipiperidinopyrimidino[5,4-d]pyrimidine serving as dipyridamole intermediate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0084] (1) Put in 110g of acetone (recovered acetone + industrial acetone), start stirring, add 30g of tetrachloride, and stir for 5-10 minutes.

[0085] (2) Add dropwise a mixture of 24.0 g of piperidine at 25-35°C. The mass ratio of piperidine to acetone is 1:1. After the addition, the natural temperature makes it react for 20 minutes (the test material is acidic, indicating that the first segment of the reaction is over).

[0086] (3) Add 18g of alkali mixture dropwise to control PH=7~8. After adding, stir at natural temperature for 15 minutes.

[0087] (4) Add 180 g of acetone to the thick liquid reaction solution, stir for 5 minutes, and filter with suction. Acetone is recovered from the mother liquor, and the filter cake is washed with water.

[0088] (5) The obtained filter cake is alternately washed with 30% acid in mass fraction and sufficient water, then filtered and washed with water to obtain 30.6 dichlorides. The content of dichloro was calculated to be 99.83%...

Embodiment 2

[0090] (1) Put in 110g of acetone (recovered acetone + industrial acetone), start stirring, add 30g of tetrachloride, and stir for 5-10 minutes.

[0091] (2) Add dropwise a mixture of 24.0 g of piperidine at 25-35°C. The mass ratio of piperidine to acetone is 1:1. After the addition, the natural temperature makes it react for 20 minutes (the test material is acidic, indicating that the first segment of the reaction is over).

[0092] (3) Add 18g of alkali mixture dropwise to control PH=7~8. After adding, stir at natural temperature for 15 minutes.

[0093] (4) Add 180 g of acetone to the thick liquid reaction solution, stir for 5 minutes, and filter with suction. Acetone is recovered from the mother liquor, and the filter cake is washed with water.

[0094] (5) The obtained filter cake is alternately washed with 30% acid in mass fraction and sufficient water, then filtered and washed with water to obtain 31.5 dichlorides. The content of dichloro was calculated to be 95.92%...

Embodiment 3

[0096] To simulate the production environment in the case of mass production and increase the amount of feed, the steps are as follows:

[0097] (1) Put in 110g of acetone (recovered acetone + industrial acetone), start stirring, add 50g of tetrachloride, and stir for 5-10 minutes.

[0098] (2) Add dropwise a mixture of 40.0 g of piperidine at 25-35°C. The mass ratio of piperidine to acetone is 1:1. After the addition, the natural temperature makes it react for 20 minutes (the test material is acidic, indicating that the first segment of the reaction is over).

[0099] (3) Add 30g of alkali mixture dropwise to control pH=7~8. After adding, stir at natural temperature for 15 minutes.

[0100] (4) Add 180 g of acetone to the thick liquid reaction solution, stir for 5 minutes, and filter with suction. Acetone is recovered from the mother liquor, and the filter cake is washed with water.

[0101] (5) The obtained filter cake is alternately washed with 30% acid in mass fraction...

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Abstract

The invention provides a refining method for 2,6-dichloro-4,8-dipiperidinopyrimidino[5,4-d]pyrimidine serving as a dipyridamole intermediate, and belongs to the field of chemical synthesis. The refining method includes the steps of putting, stirring, pH adjusting for second-stage reacting, acetone sucking filtering and recycling, filtered-cake washing and pickling and the like. As the material ratio and reaction conditions of the temperature, the pH and the like are accurately controlled in the reacting process, the number of side reactions is small, the yield of synthesized products is high, the number of the side reactions is small, the quantity of impurities is small, and purification is easy; solutions of the products are clear or in slight milk white, and compared with the traditional synthetic technology, appearance is better.

Description

technical field [0001] The invention relates to the field of chemical synthesis, in particular to a method for refining a dipyridamole intermediate 2,6-dichloro-4,8-dipiperidino-pyrimido[5,4-D]pyrimidine. Background technique [0002] Dipyridamole, also known as dipyridamole, dipyridamole, dipyridamole, is a non-nitrate coronary artery dilator, which can expand coronary blood vessels, promote the formation of collateral circulation and mildly anticoagulant. The role of the virus. Dichloride, Chinese name: 2,6-dichloro-4,8-dipiperidine (5,4d) pyrimidine, English name: DICHLORO-DIPIPERIDINEHOMOPURINE, DDH for short, is a pharmaceutical intermediate for the manufacture of dipyridamole. [0003] The current DDH synthesis process cannot meet the requirements of subsequent fine pharmaceuticals due to its extensive process, many side reactions, high impurity content in the synthetic product, and poor appearance and color of the product. [0004] In view of this, the present inven...

Claims

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Application Information

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IPC IPC(8): C07D487/04
CPCC07D487/04
Inventor 董小林赵万祥刘爱荣
Owner 芮城县虹桥药用中间体有限公司
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