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A kind of synthetic technique that improves the yield of gliclazide intermediate 2 carboxamide cyclohexanone

A synthesis process and cyclohexanone technology are applied in the field of synthesis technology for improving the yield of gliclazide intermediate 2-formamide cyclohexanone, and can solve the problems of many by-products, poor quality, low yield and the like, Achieve high product quality, reduced impurities and fewer by-products

Active Publication Date: 2017-03-15
JIANGSU RUIKE MEDICAL SCI & TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

It mainly has problems such as low yield, many by-products, and poor quality.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Add xylene and excess urea in the reaction bottle, and add a new catalyst tetraisopropyl titanium oxide with a molar weight of 4.5% cyclohexanone, control the reaction temperature at -20°C, add cyclohexanone dropwise, and the dropwise addition time is about 2 Hours, complete, keep at -20°C to -15°C for 16 hours, and control the end point of the reaction by TLC detection. After the reaction, control the temperature below 20°C, add a certain amount of water, stir for 30 minutes, let it stand for 1 hour, separate the water layer, and then extract it with water twice to complete. Recover xylene under reduced pressure to dryness, add 95% ethanol and 20% sodium carbonate solution, stir evenly, keep warm at -5°C to 0°C for 1 hour, filter, decompress the filter cake to -0.09mpa, and dry to dryness to obtain Glicazide intermediate 2-carboxamide cyclohexanone, yield 89.05%.

Embodiment 2

[0023] Add xylene and excess urea in the reaction flask, and add a new catalyst tetraisopropyltitanium oxide with a molar weight of 5% cyclohexanone, control the reaction temperature at -20°C, add cyclohexanone dropwise, and the dropwise addition time is about 2 Hours, complete, keep at -20°C to -15°C for 16 hours, and control the end point of the reaction by TLC detection. After the reaction, control the temperature below 20°C, add a certain amount of water, stir for 30 minutes, let it stand for 1 hour, separate the water layer, and then extract it with water twice to complete. Recover xylene under reduced pressure to dryness, add 95% ethanol and 20% sodium carbonate solution, stir evenly, keep warm at -5°C to 0°C for 1 hour, filter, decompress the filter cake to -0.09mpa, and dry to dryness to obtain Glicazide intermediate 2-carboxamide cyclohexanone, yield 90.44%.

Embodiment 3

[0025] Add xylene and excess urea to the reaction flask, and add a new catalyst tetraisopropyl titanium oxide with a molar weight of 5.5% cyclohexanone, control the reaction temperature at -20°C, add cyclohexanone dropwise, and the dropwise addition time is about 2 Hours, complete, keep at -20°C to -15°C for 16 hours, and control the end point of the reaction by TLC detection. After the reaction, control the temperature below 20°C, add a certain amount of water, stir for 30 minutes, let it stand for 1 hour, separate the water layer, and then extract it with water twice to complete. Recover xylene under reduced pressure to dryness, add 95% ethanol and 20% sodium carbonate solution, stir evenly, keep warm at -5°C to 0°C for 1 hour, filter, filter the cake under reduced pressure to -0.09mpa, and then dry to dryness to obtain Glicazide intermediate 2-carboxamide cyclohexanone, yield 90.25%.

[0026] Of course, other steps in the intermediate synthesis production process of this m...

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Abstract

The invention provides a synthesizing process for improving the yield of a gliclazide intermediate 2-formamide cyclohexanone. According to the invention, on the basis of an original process, a novel catalyst titanium(IV) isopropoxide is added into a reaction system, such that a synthesis yield is improved from 82% to 90% while product quality is improved. The process has significant economic benefits.

Description

technical field [0001] The invention relates to a synthesis process of a gliclazide intermediate, in particular to a synthesis process of 2-carboxamide cyclohexanone. Background technique [0002] Gliclazide is a second-generation sulfonylurea hypoglycemic drug with a strong effect, and its mechanism is to selectively act on pancreatic β cells to promote insulin secretion. Through the insulin receptor mechanism, it increases the activity of glycogen synthase in bones, promotes the utilization of glucose by muscles, and can reduce the aggregation and adhesion of platelets, which helps prevent and treat diabetic microangiopathy. [0003] The existing gliclazide intermediate 2-carboxamide cyclohexanone synthesis process uses ethyl acetate as the reaction solvent, and it is obtained by condensation with urea and cyclohexanone under anhydrous conditions, distillation, water crystallization, filtration, and drying . It mainly has problems such as low yield, many by-products, and...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C235/82C07C231/10
Inventor 赵小泉朱家伍张杰
Owner JIANGSU RUIKE MEDICAL SCI & TECH CO LTD