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Method for preparing purine derivatives

A compound and reaction mixture technology, applied in the field of preparation of purine derivatives, can solve the problem of high reaction temperature

Inactive Publication Date: 2015-03-04
SUNSHINE LAKE PHARM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In these methods, there are problems such as the need to use column chromatography for separation and purification or high reaction temperature

Method used

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  • Method for preparing purine derivatives
  • Method for preparing purine derivatives
  • Method for preparing purine derivatives

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Experimental program
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specific Embodiment approach

[0030] In order to enable those skilled in the art to better understand the technical solutions of the present invention, some non-limiting examples are further disclosed below to further describe the present invention in detail.

[0031] The reagents used in the present invention can be purchased from the market or can be prepared by the methods described in the present invention.

[0032] In the present invention, g means gram, and mL means milliliter.

Embodiment 1

[0034] Add 150 mL of dimethyl sulfoxide, 10 g of compound (01), 7.13 g of compound (02), 9.30 g of potassium carbonate, and 0.61 g of tetrabutylammonium bromide into the reaction flask. The temperature was raised to 60° C. under stirring, and reacted for 6 hours to obtain the first reaction liquid. Add 8.2 g of compound (03) to the first reaction liquid, raise the temperature to 75°C-80°C and react for 16 hours, and the reaction is completed. 200mL of water was added dropwise to the reaction system, and after the dropwise addition, the temperature was lowered to 25°C and stirred for 2 hours; filtered, and the resulting solid was vacuum-dried at 45°C to obtain compound (II): 18.09g, purity: 97.5%.

Embodiment 2

[0036] Add 100 mL of N-methylpyrrolidone, 10.00 g of compound (01), 7.70 g of compound (02), 9.55 g of potassium carbonate, and 1.87 g of tetrabutylammonium chloride into the reaction flask. The temperature was raised to 65° C.-70° C. under stirring, and reacted for 4 hours to obtain the first reaction solution. Add 7.45 g of compound (03) to the first reaction liquid, raise the temperature to 80°C-85°C and react for 13 hours, and the reaction ends. Add 200mL of water dropwise to the reaction system. After the dropwise addition, cool down to 25°C and stir for 2h; filter and dry the obtained solid under vacuum at 45°C to obtain compound (II): 17.85g, purity: 97.9%.

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Abstract

The invention provides a method for preparing an intermediate of trajenta and belongs to the technical field of pharmacy. The method comprises the following steps: reacting 8-bromo-7-(2-butynyl)-3-methyl-1-purine-2,6-dione with 2-chloromethyl-4-methylquinazoline to obtain a reaction liquid; reacting the reaction liquid with (R)-3-tert-butyloxycarboryl-aminopiperidine to obtain 8-[(3R)-3-(tert-butyloxycarboryl-amino)-1-piperidyl]-7-(2-butynyl)-3,7-dihydro-3-methyl-1-[(4-methyl-2-quinazolinyl)-methyl]-1H-purine-2,6-dione. In the reacting process, an intermediate product is not separated. According to the preparation method, the intermediate product does not need to be separated or purified, the operation is simplified, the yield is high, the production cost is reduced, and the industrial production is benefited.

Description

technical field [0001] The invention relates to a preparation method of purine derivatives, belonging to the technical field of pharmacy. Background technique [0002] Linagliptin, a selective dipeptidyl peptidase IV (DPP-IV) inhibitor, can significantly control blood sugar with only once-daily oral administration, risk of hypoglycemia, cardiovascular events and weight gain Lower, the market prospect is better. Linagliptin is a purine derivative, and its compound structure contains a substituted quinazoline group and a 3-aminopiperidine group, and its structure is shown in the following formula (1): [0003] [0004] The methods disclosed in the prior art such as US20130123282 and WO2005051950 usually use a compound containing a halogenated quinazoline group to react with a halogenated purine derivative to isolate an intermediate, and then combine the isolated intermediate with a piperidine derivative reaction, and then deprotection method to obtain the final product li...

Claims

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Application Information

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IPC IPC(8): C07D473/04
CPCC07D473/04
Inventor 林碧悦肖清波寇景平
Owner SUNSHINE LAKE PHARM CO LTD
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