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Chlormezanone drug intermediate 4-chlorobenzaldehyde synthesis method

A technology of chlorobenzaldehyde and synthesis method, which is applied in the fields of oxidative preparation of carbonyl compounds, organic chemistry, etc., can solve problems such as high reaction temperature, high risk factor, and poisonous chlorine gas, and achieve low reaction temperature, lower risk factor, and high reaction yield Improved effect

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

But this synthesis method is too loaded down with trivial details, and the required chlorine gas is poisonous in the reaction process, and operation process risk factor is higher, and reaction temperature is higher, mostly above 150 ℃, and required energy consumption is higher, therefore need to improve and propose a new synthesis method

Method used

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  • Chlormezanone drug intermediate 4-chlorobenzaldehyde synthesis method
  • Chlormezanone drug intermediate 4-chlorobenzaldehyde synthesis method
  • Chlormezanone drug intermediate 4-chlorobenzaldehyde synthesis method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] The synthetic method of fenalu pharmaceutical intermediate 4-chlorobenzaldehyde comprises the steps:

[0016] Add 2-methyl-3-bromo-5-chlorophenol of 2.5mol, 3mol mass fraction and be 80% 4-methyl-2-pentanone solution in the reaction vessel, control stirring speed 170rpm, raise solution temperature to 40°C, add 3.2mol molybdenum pentachloride powder in 3 times, continue to react for 40min after addition, 1.32kPa vacuum distillation, collect 82°C fraction, wash in 80% butyl oxalate solution for 3 Washing 5 times in 85% ethanedinitrile solution and recrystallizing in 90% 2-methylbutyric acid solution gave 311.5 g of crystalline 4-chlorobenzaldehyde with a yield of 89%.

Embodiment 2

[0018] The synthetic method of fenalu pharmaceutical intermediate 4-chlorobenzaldehyde comprises the steps:

[0019] Add 2.5mol of 2-methyl-3-bromo-5-chlorophenol and 3.3mol mass fraction of 84% 4-methyl-2-pentanone solution in the reaction vessel, control the stirring speed to 190rpm, and raise the solution temperature To 45°C, add 3.4mol molybdenum pentachloride powder in 5 times, continue to react for 45min after addition, 1.34kPa vacuum distillation, collect 83°C fraction, wash in 83% butyl oxalate solution 5 times, washed 6 times in 87% ethanedinitrile solution, and recrystallized in 93% 2-methylbutyric acid solution to obtain 322 g of crystalline 4-chlorobenzaldehyde with a yield of 92%.

Embodiment 3

[0021] The synthetic method of fenalu pharmaceutical intermediate 4-chlorobenzaldehyde comprises the steps:

[0022] Add 2.5mol of 2-methyl-3-bromo-5-chlorophenol and 3.6mol mass fraction of 87% 4-methyl-2-pentanone solution in the reaction vessel, control the stirring speed to 210rpm, and raise the solution temperature To 49°C, add 3.4mol molybdenum pentachloride powder in 6 times, continue to react for 50min after the addition, 1.36kPa vacuum distillation, collect the fraction at 84°C, wash in 86% butyl oxalate solution 5 times, washed 6 times in ethanedinitrile solution with a mass fraction of 91%, and recrystallized in a 2-methylbutyric acid solution with a mass fraction of 96%, to obtain 329 g of crystalline 4-chlorobenzaldehyde with a yield of 94%.

[0023] Finished product 4-chlorobenzaldehyde is done infrared analysis, and infrared spectrogram is as follows figure 1 Shown, Table 1 is the analysis data.

[0024] Table 1 Spectrum peak data table

[0025]

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Abstract

The invention discloses a chlormezanone drug intermediate 4-chlorobenzaldehyde synthesis method, which mainly comprises: adding 2-methyl-3-bromo-5-chlorophenol and a 4-methyl-2-pentanone solution to areaction container, controlling the stirring speed, increasing the temperature of the solution, adding molybdenum pentachloride powder in batches, continuously carrying out the reaction after completing the adding, carrying out pressure reducing distillation, washing the obtained distillate multiple times in a butyl valerate solution, washing multiple times in a cyanogen solution, and re-crystallizing in a 2-methylbutyric acid solution to obtain the crystal 4-chlorobenzaldehyde.

Description

technical field [0001] The invention relates to a method for preparing medicine, which belongs to the field of organic synthesis, and in particular to a method for synthesizing 4-chlorobenzaldehyde, a pharmaceutical intermediate of fenarol. Background technique [0002] 4-Chlorobenzaldehyde is mainly used in the manufacture of pharmaceutical raw materials and intermediates such as sedatives such as fennarol and phenylbutyric acid, and in the manufacture of chlorocinnamaldehyde and weed killing powder in pesticides. Fenarol can be used as a weak tranquilizer. It has sedative, stable and central muscle relaxation effects. It can also be used for mental stress and fear, chronic fatigue, anxiety, excitement, and irritability and insomnia caused by certain diseases. Because of its muscle relaxation effect, it can be used with analgesics for backache, stiff neck, bone pain, spine and limb pain, and rheumatic joint pain. The existing synthesis method often uses p-chlorotoluene o...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C45/28C07C47/55
CPCC07C45/28C07C47/55
Inventor 彭飞
Owner CHENGDU QIESITE TECH CO LTD
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