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Synthesis method of perhexiline drug intermediate alpha-(2,2-diphenyl vinyl) pyridine

A technology of diphenylethylene and perhexiline, which is applied in the field of synthesis of perhexiline pharmaceutical intermediate α-pyridine, can solve problems such as aggravation of myocardial ischemia, reduce intermediate links, improve reaction yield, reduce Effect of reaction temperature and reaction time

Inactive Publication Date: 2016-04-20
CHENGDU QIANYE LONGHUA PETROLEUM ENG TECH CONSULTING
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Benefits of technology

This technology reduces intermediates between reactants while improving their efficiency at lower temperatures or longer times compared with previous methods like batch reactions.

Problems solved by technology

The technical problem addressed in this patented text is that current treatments like vasospasm suppression have limitations such as causing damage caused by excessively high levels of calcium leading to periphery necrosis and decreased blood supply from brain tissue. This results in reduced ability to open up blocked veins and improve blood circulation while minimizing negative symptoms associated therewith.

Method used

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  • Synthesis method of perhexiline drug intermediate alpha-(2,2-diphenyl vinyl) pyridine

Examples

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Effect test

example 1

[0011] In a reaction vessel equipped with a stirrer, a reflux condenser, a thermometer and a dropping funnel, add 1,1-diphenyl-2-(α-pyridyl)ethylamine (2) 1.56mol, with a mass fraction of 30% Phenyl hypochlorite solution (3) 1.81mol, 300ml of nitromethane, control the stirring speed to 150rpm, raise the temperature of the solution to 80°C, react for 3h, lower the temperature of the solution to 45°C, add 20% potassium carbonate solution to adjust The pH was 9, the reaction was continued to stir for 5h, the temperature of the solution was lowered to 10°C, a solid was precipitated, suction filtered, washed with ammonium nitrate solution, washed with 50% chlorobenzene, decolorized by molecular sieve, stirred and refluxed for 3h, dehydrated with anhydrous potassium carbonate, The mass fraction was 90% of p-xylene and recrystallized to obtain 276.63 g of crystalline α-(2,2-diphenylvinyl)pyridine with a yield of 69%.

example 2

[0013] In a reaction vessel equipped with a stirrer, a reflux condenser, a thermometer and a dropping funnel, add 1,1-diphenyl-2-(α-pyridyl)ethylamine (2) 1.56mol, with a mass fraction of 32% Phenyl hypochlorite solution (3) 1.9mol, nitromethane 300ml, control the stirring speed to 170rpm, raise the solution temperature to 82°C, react for 4h, lower the solution temperature to 47°C, add a mass fraction of 23% potassium carbonate solution to adjust The pH was 9, the reaction was continued to stir for 6h, the temperature of the solution was lowered to 12°C, the solid was precipitated, filtered with suction, washed with potassium iodide solution, washed with 52% chlorobenzene, decolorized by molecular sieve, stirred and refluxed for 3h, dehydrated with activated alumina, at the mass fraction It was recrystallized from 92% p-xylene to obtain 292.67 g of crystalline α-(2,2-diphenylvinyl)pyridine with a yield of 73%.

example 3

[0015] In a reaction vessel equipped with a stirrer, a reflux condenser, a thermometer and a dropping funnel, add 1,1-diphenyl-2-(α-pyridyl)ethylamine (2) 1.56mol, with a mass fraction of 35% Phenyl hypochlorite solution (3) 2.1mol, 300ml of nitromethane, control the stirring speed to 190rpm, raise the temperature of the solution to 85°C, react for 5h, lower the temperature of the solution to 50°C, add 25% potassium carbonate solution to adjust The pH was 10, the reaction was continued to stir for 7h, the temperature of the solution was lowered to 15°C, a solid was precipitated, suction filtered, washed with ammonium nitrate solution, washed with 55% chlorobenzene, decolorized by molecular sieve, stirred and refluxed for 4h, dehydrated with anhydrous potassium carbonate, The mass fraction was 95% p-xylene and recrystallized to obtain 312.72 g of crystalline α-(2,2-diphenylvinyl)pyridine with a yield of 78%.

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Abstract

A synthesis method of a perhexiline drug intermediate alpha-(2,2-diphenyl vinyl) pyridine includes the following steps that 1.56 mol of 1,1-diphenyl-2-(alpha-pyridyl) ethylamine, 1.8-2.1 mol of a hypochlorous phenyl ester solution and 300 ml of nitromethane are added into a reaction vessel provided with a stirrer, a reflux condenser, a thermometer and a dropping funnel, the stirring speed is controlled to be 150-190 rpm, the solution temperature is raised to 80-85 DEG C, reaction is performed for 3-5 hours, the solution temperature is reduced to 45-50 DEG C, a potassium carbonate solution is added to regulate the pH to 9-10, continuous stirring is performed for reaction for 5-7 hours, the solution temperature is reduced to 10-15 DEG C, solid precipitation, suction filtration, washing with a saline solution, washing with chlorobenzene and decoloration with a molecular sieve are performed, stirring reflux is performed for 3-4 hours, a dehydrating agent is adopted fordehydration, and recrystallization is performed in p-xylene to obtain the crystal alpha-(2,2-diphenyl vinyl) pyridine.

Description

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Claims

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Application Information

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Owner CHENGDU QIANYE LONGHUA PETROLEUM ENG TECH CONSULTING
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