Method for preparing p-tert-butylbenzylamine

A technology of p-tert-butylbenzylamine and p-tert-butylbenzyl chloride, applied in the field of compound preparation, can solve the problems of inability to obtain tert-butylbenzylamine and low purity

Inactive Publication Date: 2010-05-12
HUAZHONG AGRI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

To overcome the large amount of impurities that exist in the p-tert-butylbenzylamine prepared by the existin

Method used

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  • Method for preparing p-tert-butylbenzylamine
  • Method for preparing p-tert-butylbenzylamine
  • Method for preparing p-tert-butylbenzylamine

Examples

Experimental program
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Effect test

Embodiment 1

[0016] Embodiment 1 (control test, does not carry out secondary hydrolysis)

[0017] Add 5.7g of urotropine and 15ml of chloroform into a 250ml three-necked flask, set up a condensation reflux device, a thermometer, and stir at room temperature. The wall of the bottle was washed with chloroform, and the reaction was refluxed at 62° C. for 1 h. After the reaction is complete, a large amount of white solid precipitates are produced, cooled to room temperature, and suction filtered to obtain the white solid, which is the hexatropine quaternary ammonium salt of p-tert-butylbenzyl chloride prepared by the present invention;

[0018] The white solid obtained in the above steps is transferred to a 250ml three-necked flask, 15ml of concentrated hydrochloric acid is added thereto, it is dissolved under stirring, and then 45ml of ethanol with a concentration of 95% is slowly added, a large amount of white solid precipitates appear, and continue to dissolve at 80 Reflux reaction at ℃ fo...

Embodiment 2

[0020] Embodiment 2 (the present invention)

[0021] Add 5.7g of urotropine and 15ml of chloroform into a 250ml three-necked flask, set up a condensation reflux device, a thermometer, and stir at room temperature. After the urotropine is fully dissolved, add 6.1g of p-tert-butylbenzyl chloride at one time , and then rinse the bottle wall with 5ml chloroform, and heat and reflux at 62°C for 1h. After the reaction is completed, a large amount of white solid precipitates are produced, cooled to room temperature, and the white solid is obtained by suction filtration, which is the quaternary ammonium salt of tert-butyl benzyl chloride. ;

[0022] The white solid obtained in the above steps is transferred to a 250ml three-necked flask, 15ml of concentrated hydrochloric acid is added thereto, it is dissolved under stirring, and then 45ml of ethanol with a concentration of 95% is slowly added, a large amount of white solid precipitates appear, and continue to dissolve at 80 Reflux at...

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Abstract

The invention belongs to the technical field of compound preparation and discloses a chemical synthetic method for preparing p-tert-butylbenzylamine. The chemical synthetic method is characterized by comprising the following steps: firstly, reacting p-tert-butylbenz with urotropine to prepare quaternary ammonium salt, carrying out prehydrolysis on the quaternary ammonium salt by hydrochloric acid and alcohol solution, filtering, evaporating a solvent to obtain p-tert-butylbenzylamine hydrochloride solid; using the p-tert-butylbenzylamine hydrochloride solid as a raw material, using hydrochloric acid and water to carry out secondary hydrolysis on the p-tert-butylbenzylamine hydrochloride solid, reducing pressure, evaporating the solution to be dried, obtaining faint yellow solid matter, and using 40 percent sodium hydroxide solution to adjust pH of the faint yellow solid matter to be 8 to 12, thus obtaining the p-tert-butylbenzylamine. The chemical synthetic method can effectively remove a large amount of impurities in the p-tert-butylbenzylamine prepared by the existing method and obtain the p-tert-butylbenzylamine with high purity.

Description

technical field [0001] The invention belongs to the technical field of compound preparation, and in particular relates to a chemical synthesis method of p-tert-butylbenzylamine. The compound p-tert-butylbenzylamine is an important intermediate for synthesizing drugs such as the new acaricide tebufenpyrad. Background technique [0002] 4-tert-butylbenzylamine is a bright yellow transparent liquid with a boiling point of 115°C to 118°C at a vacuum of 20 mmHg. P-tert-butylbenzylamine is an important pesticide, a pharmaceutical intermediate, and an important intermediate for the synthesis of drugs such as the new acaricide tebufenpyrad and dopamine receptor agonists (Gu Baoquan et al. Synthesis of tebufenpyrad[J].Modern Pesticides, 2002, (6): 9-11.) and dopamine receptor agonists (Nelson J A, Mewshaw R E, Shah US.4-Amino-alkoxy-1, 3-dihydrobenzoimidazol-2-one dopamine autoreceptor agonists[P] . US 5990144, 1999). [0003] The chemical synthesis method of p-tert-butylbenzylamin...

Claims

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Application Information

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IPC IPC(8): C07C211/27C07C209/62
Inventor 江洪林创业韩鹤友方志勇
Owner HUAZHONG AGRI UNIV
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