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Method for producing 1-p-methylphenyl ethylamine

A technology of tolylethylamine and p-methylacetophenone, applied in the production of chemical intermediates and the production of intermediate 1-p-tolylethylamine, which can solve the problems of harsh ultra-high pressure conditions, high equipment requirements, and poor safety , to achieve the effect of cheap raw materials, good safety, and low equipment requirements

Inactive Publication Date: 2011-05-04
江苏八巨药业有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] Although this method uses low-priced and easy-to-buy raw materials and has few reaction steps, the reaction requires ultra-high pressure conditions, high requirements for equipment, and poor safety.

Method used

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  • Method for producing 1-p-methylphenyl ethylamine
  • Method for producing 1-p-methylphenyl ethylamine
  • Method for producing 1-p-methylphenyl ethylamine

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] In the 500ml there-necked flask equipped with stirrer, thermometer, reflux cooler, drop into raw material 44.5g p-methyl acetophenone, 27.6 gram hydroxylamine hydrochloride, mixed solvent 140g ethanol and 10g water. Add 24g of neutralizing agent sodium hydroxide under the condition of stirring, and finish the dosage in 5 times. Cool to room temperature, add 320ml of water, cool to below 5°C with stirring and filter quickly, and dry the filter cake at about 50°C to obtain the oximate with a yield greater than 95%.

[0034] Put the oximide prepared above, 500ml of anhydrous methanol and 4gW-2 Raney nickel into the pressure vessel, and then pass hydrogen to maintain the pressure of the reaction system at 1.2-1.3Mpa, the temperature is 70°C, and the catalytic hydrogenation reaction time is about After 4 hours, the end point was detected by TLC, and a catalytic hydrogenation material containing crude 1-p-tolylethylamine was obtained after the reaction.

[0035] The catalyti...

Embodiment 2

[0037] The device used for the oximation reaction is the same as in Example 1, and will not be described in detail; 89g of p-methylacetophenone, 52.1g of hydroxylamine sulfate, 192g of ethanol and 60g of water as the mixed solvent are put into the raw material. Add 46g of neutralizing agent sodium hydroxide under the condition of stirring, and finish the dosage in 6 times. Cool to room temperature, add 480ml of water, cool to below 5°C with stirring and quickly filter, and quickly dry the filter cake at about 50°C to obtain the oximide with a yield greater than 95%.

[0038]Put the oximide prepared above, 600ml of anhydrous methanol and 2g of platinum oxide into the pressure vessel, and then pass hydrogen to maintain the pressure of the reaction system at 1.4-1.6Mpa, the temperature is 60°C, the catalytic hydrogenation reaction time is about 5 hours, TLC The end point is detected, and the catalytic hydrogenation material containing the crude product of 1-p-tolylethylamine is o...

Embodiment 3

[0041] The device used for the oximation reaction is the same as in Example 1, and will not be described in detail; 92g of p-methylacetophenone, 54g of hydroxylamine hydrochloride, 185g of ethanol and 55g of water as a mixed solvent are put into the raw materials. Put in 48g of neutralizing agent sodium hydroxide under the condition of stirring, divide into 5 times, control the temperature at 40-45°C, heat to 70°C and reflux for 6 minutes after the throwing, after the reaction, distill and recover ethanol under normal pressure conditions, Cool to room temperature, add 500ml of water, cool to below 5°C with stirring, and quickly filter, and dry the filter cake at about 50°C to obtain the oximate, with a yield of up to 90%.

[0042] Put the oximide prepared above, 800ml of anhydrous methanol and 3g of palladium carbon into the pressure vessel, and then pass hydrogen to maintain the pressure of the reaction system at 1.6-1.8Mpa, the temperature is 80°C, the catalytic hydrogenation...

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Abstract

The invention relates to a production method of intermediate 1-p-methylphenyl ethylamine, belonging to the medical and chemical technical field, which comprises oximation reaction, catalytic hydrogenation reaction and following treatment or the like. The invention resolves the problems of prior production method of intermediate 1-p-methylphenyl ethylamine which has high demand on device, needs ultrahigh pressure and low safety. The inventive production method of 1-p-methylphenyl ethylamine has cheap and easily accessible material, low cost, high product yield, high product purity, few reaction steps and high safety.

Description

technical field [0001] The invention relates to a method for producing a chemical intermediate, in particular to a method for producing the intermediate 1-p-tolylethylamine; it belongs to the technical fields of medicine and chemical industry. Background technique [0002] 1-p-tolylethylamine is an important intermediate of medicine, pesticide and dyestuff, it can be synthesized by many methods, but from the production cost, the simplicity of the technological process, the number of reaction steps, the ease of purchase and cost of raw materials and Factors such as the degree of intensity of the whole reaction process are considered, and generally many take p-methylacetophenone as raw material, and its preparation method mainly contains following two kinds: [0003] Method 1: Using p-methyl acetophenone as raw material, react it with ammonium formate to obtain N-p-tolylethyl formamide, acidify and hydrolyze to obtain N-p-tolylethylamine hydrochloride, and then alkali hydrolyz...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C211/27C07C209/40
Inventor 徐斌程锦涛陈斌吴六君李炳全郦观江陈恬
Owner 江苏八巨药业有限公司
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