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Vitamin K3 drug intermediate 2-menaquinone synthesis method

A synthetic method and vitamin technology, applied in the synthesis of vitamin K3 drug intermediate 2-menadione, and the field of preparation of pharmaceutical intermediates, can solve the problems of complex process, large environmental pollution, high reaction energy consumption, etc., to achieve improved reaction yield The effect of low reaction energy consumption and high reaction yield

Inactive Publication Date: 2018-07-03
CHENGDU QIESITE TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, this synthesis method requires chromic acid as a reactant, which is more polluting to the environment, and the reaction process requires a high temperature of 110 ° C, the reaction energy consumption is high, and the process is more complicated. Therefore, it is necessary to propose a new synthesis method

Method used

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  • Vitamin K3 drug intermediate 2-menaquinone synthesis method
  • Vitamin K3 drug intermediate 2-menaquinone synthesis method
  • Vitamin K3 drug intermediate 2-menaquinone synthesis method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] The synthetic method of vitamin K3 drug intermediate 2-menadione, comprises the steps:

[0019] A. Add 3mol of 1,4-dihydroxy-2-methylnaphthalene to the reaction vessel, 1.6L mass fraction of 10% potassium chloride solution, increase the temperature of the solution to 45°C, control the stirring speed at 260rpm, add 3mol of The mass fraction is 30% acetylacetone solution, reacted for 90 minutes;

[0020] B. Add 2 mol of thulium oxide in 3 times within 40 minutes, increase the solution temperature to 55°C, react for 60 minutes, add 1.3L of potassium sulfate solution with a mass fraction of 25%, lower the temperature to 10°C, let stand to separate layers, add mass The fraction is 15% oxalic acid solution, adjust the pH to 5, wash with 50% 3-chloro-1-propanol solution, 60% chlorohexane solution, and 85% sulfuryl chloride Recrystallized in the solution and dehydrated with anhydrous calcium sulfate dehydrating agent to obtain 459.24 g of finished product 2-menaquinone with a ...

Embodiment 2

[0022] The synthetic method of vitamin K3 drug intermediate 2-menadione, comprises the steps:

[0023] A. Add 3mol of 1,4-dihydroxy-2-methylnaphthalene to the reaction vessel, 1.6L mass fraction of 13% potassium chloride solution, raise the temperature of the solution to 47°C, control the stirring speed to 280rpm, add 3.5mol A solution of acetylacetone with a mass fraction of 35%, reacted for 110 minutes;

[0024] B. Add 2.5 mol of thulium oxide in 5 times within 50 minutes, increase the solution temperature to 57°C, react for 80 minutes, add 1.3L of potassium sulfate solution with a mass fraction of 27%, lower the temperature to 13°C, let stand and separate, Add grass mass fraction as 18% oxalic acid solution, adjust pH to 5.5, wash with 3-chloro-1-propanol solution with mass fraction of 55%, and wash with chlorohexane solution with mass fraction of 65%. % recrystallized in sulfuryl chloride solution and dehydrated with anhydrous potassium carbonate dehydrating agent to obta...

Embodiment 3

[0026] The synthetic method of vitamin K3 drug intermediate 2-menadione, comprises the steps:

[0027] A. Add 3mol of 1,4-dihydroxy-2-methylnaphthalene to the reaction vessel, 1.6L mass fraction of 16% potassium chloride solution, increase the temperature of the solution to 50°C, control the stirring speed at 290rpm, and add 4mol mass Fraction is 37% acetylacetone solution, react for 120min;

[0028] B. Add 3 mol of thulium oxide in 6 times within 60 minutes, increase the temperature of the solution to 60°C, react for 90 minutes, add 1.3L of 30% potassium sulfate solution by mass fraction, lower the temperature to 16°C, let stand for stratification, and add the mass fraction 21% oxalic acid solution, adjust pH to 6, wash with 58% 3-chloro-1-propanol solution, 67% chlorohexane solution, and 90% sulfuryl chloride solution Medium recrystallization, dehydration with phosphorus pentoxide dehydrating agent, 495.36 g of finished product 2-menadione was obtained, yield 96%.

[0029]...

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Abstract

The invention discloses a vitamin K3 drug intermediate 2-menaquinone synthesis method, which comprises: adding 1,4-dihydroxy-2-methyl naphthalene and a potassium chloride solution in a reaction container, increasing the temperature of the solution, controlling the stirring speed, adding an acetylacetone solution, carrying out a reaction, adding thulium oxide in batches, increasing the temperatureof the solution, carrying out a reaction for 60-90 min, adding a potassium sulfate solution, reducing the temperature to 10-16 DEG C, carrying out standing layering, adding an oxalic acid solution, adjusting the pH value to 5-6, washing with a 3-chloro-1-propanol solution, washing with a chlorohexane solution, re-crystallizing in a sulfuryl chloride solution, and dehydrating with a dehydrating agent to obtain the finished product 2-menaquinone.

Description

technical field [0001] The invention relates to a preparation method of a pharmaceutical intermediate, belonging to the field of organic synthesis, in particular to a synthesis method of vitamin K3 pharmaceutical intermediate 2-menadione. Background technique [0002] 2-Menadione mainly promotes the synthesis of prothrombin in the liver of livestock and poultry, and promotes the synthesis of plasma coagulation factors in the liver. It is a hemostatic agent and can be used as a vitamin K3 drug intermediate. Most of the existing synthetic methods adopt the cyclization of toluoquinone and butadiene to obtain 2-methylnaphthohydroquinone, which is then oxidized by chromic acid. Add toluquinone to dissolve in glacial acetic acid, pass through butadiene, and pass through to the required amount below 20°C. After airtight and standing for 20 hours, heat to escape the remaining butadiene, continue heating to about 110°C and reflux for 3 hours, and then recover about 30% of glacial ac...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C46/06C07C46/10C07C50/12
CPCC07C46/06C07C46/10C07C50/12
Inventor 彭飞
Owner CHENGDU QIESITE TECH CO LTD
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