Preparation method for Trajenta

A compound and preset temperature technology, applied in the direction of organic chemistry, can solve the problems of unfavorable industrial production, no large-scale production, high cost, etc., and achieve the effect of meeting the needs of industrial production, low production cost, and avoiding dimer impurities

Active Publication Date: 2015-06-03
CHINA RESOURCES SAIKE PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Benefits of technology

This patented technology provides an improved way to make linderspeptide with fewer unwanted side products that improve its quality compared to existing methods such as chemical synthesis or enzymatic reactions.

Problems solved by technology

This patented technical problem addressed in this patents relates to improving the efficiency of making liacreturtodina from linagridone without generating unwanted side products or contaminating other materials during manufacturing processes due to poor quality control over both chemical reactions involved.

Method used

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  • Preparation method for Trajenta
  • Preparation method for Trajenta
  • Preparation method for Trajenta

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0048]

[0049] Step 1: Add 10.0g of compound a, 8.0g of compound b, and 7.0g of potassium carbonate into 100mL of N-methylpyrrolidone in turn, stir and heat up to 120°C for reaction, monitor by TLC, after the reaction is complete, cool down to 20°C, and dissolve the reaction solution Poured into 500mL of purified water, precipitated solid, filtered, and air-dried at 45°C to obtain compound c with a mass of 11.5g;

[0050] Step two:

[0051]

[0052] Add 5.0g of compound c to 25mL of dichloromethane, add 15mL of trifluoroacetic acid pretreated by distillation, react at 20°C, and monitor by TLC. After the reaction is complete, add 100mL of dichloromethane and 200mL of water to the reaction solution in sequence, Stir for 1 hour, separate the layers, wash the water layer once with 50 mL of dichloromethane, separate the layers, add 100 mL of dichloromethane again to the water layer, adjust the pH to 10-11 with 20% by mass sodium hydroxide solution, and separate the layers ,...

Embodiment 2

[0059]

[0060] Step 1: Add 2.0g of compound a, 2.0g of compound b, and 1.4g of potassium carbonate into 20mL of N,N-dimethylformamide in turn, stir and heat up to about 110°C for reaction, monitor by TLC, after the reaction is complete, cool down to 30°C ℃, pour the reaction liquid into 100mL of purified water, precipitate solid, filter, and blow dry at 45℃ to obtain compound c with a mass of 2.1g;

[0061] Step two:

[0062]

[0063] Add 5.0g of compound c to 25mL of dichloromethane, add 15mL of trifluoroacetic acid / dichloromethane solution pretreated by distillation, react at 10°C, monitor by TLC, after the reaction is complete, add 100mL of dichloromethane to the reaction solution in turn and 200mL of water, stirred at room temperature for 1h, separated, the water layer was washed once with 50mL of dichloromethane, separated, and 100mL of dichloromethane was added to the water layer again, and the pH was adjusted to 10 with 20% sodium hydroxide solution. -11, liquid...

Embodiment 3

[0070]

[0071] Step 1: Add 2.0g of compound a, 2.7g of compound b, and 1.4g of potassium carbonate to 20mL N,N-dimethylformamide in turn, stir and heat up to about 115°C for reaction, monitor by TLC, after the reaction is complete, cool down to 25°C °C, pour the reaction solution into 100 mL of purified water, precipitate solid, filter, and blow dry at 45 °C to obtain compound c with a mass of 1.8 g;

[0072] Step two:

[0073]

[0074] Add 5.0g of compound c to 25mL of dichloromethane, add 15mL of trifluoroacetic acid / dichloromethane solution pretreated by distillation, react at 30°C, monitor by TLC, after the reaction is complete, add 100mL of dichloromethane to the reaction solution in turn and 200mL of water, stirred at room temperature for 1h, separated, the water layer was washed once with 50mL of dichloromethane, separated, and 100mL of dichloromethane was added to the water layer again, and the pH was adjusted to 10 with 20% sodium hydroxide solution. -11, liqu...

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Abstract

The invention discloses a preparation method for Trajenta. The Trajenta is a high-purity Trajenta which is prepared by taking a raw material 8-bromo-7-(2-butynyl)-3-methylxanthine, namely a compound a as basic material, selecting appreciate reaction material ratio, reaction time and reaction conditions in substitution, deprotection and other reaction steps. The preparation method has the beneficial effects that a novel method for preparing the Trajenta is provided, and dimer impurities generated in the reaction process are effectively avoided, so that the high-purity Trajenta is obtained, the raw material of the reaction are easily available, the production cost is low, and industrial production requirement of the Trajenta can be met to the greatest extent.

Description

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Claims

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Application Information

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Owner CHINA RESOURCES SAIKE PHARMA
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