Preparation method of 1, 4-dimethyl pentylamine hydrochloride

A technology of dimethylpentylamine hydrochloride and dimethylformylpentylamine, which is applied in 1 field, can solve the problems of complex preparation process, many raw material components, low yield and the like, and achieves simple preparation method and easy process control. , produce cleaning effect

Pending Publication Date: 2021-11-19
HUNAN PROVINCE HONGJIANG HUAGUANG BIOTECH
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Problems solved by technology

The preparation process is complex, the raw material components are many, and the operation steps are cumbersome. The reaction is first reduced with potassium borohydride or sodium borohydride, and then hydrogen reduction is catalyzed by palladium carbon, which involves a hydrogenation process and is not conducive to safe production.
[0004] Invention patent CN201010227035.0 discloses a synthesis method of 1,3-dimethylamylamine hydrochloride. The applicant uses its reaction conditions to verify that 5-methyl-2-hexanone is used instead of 4-methyl- 2-hexanone is amidated and hydrolyzed into a salt reaction to obtain 1,4-dimethylamylamine hydrochloride. The yield is low, and the product content is 98.2%, which cannot meet the needs of downstream users (see the specific implementation method). Comparative example 1)

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  • Preparation method of 1, 4-dimethyl pentylamine hydrochloride
  • Preparation method of 1, 4-dimethyl pentylamine hydrochloride

Examples

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preparation example Construction

[0024] A kind of preparation method of 1,4-dimethylamylamine hydrochloride, the reaction process of its preparation method is as figure 1 As shown, the specific steps are:

[0025] (1) Amidation: Use 5-methyl-2-hexanone as raw material, add reducing agent formic acid and ammonium formate while stirring, heat up to 110-115°C for 3 hours, then heat up to 130-135°C for 3 hours hours, and finally raised the temperature to 150-160° C. for 3 hours, cooled, stood to separate layers, washed, dried, and suction filtered to obtain 1,4-dimethylformyl amylamide.

[0026] (2) Hydrolysis into salt: adding the above-mentioned 1,4-dimethylformyl amylamide into hydrochloric acid with a mass concentration of 36%, heating and reflux reaction under stirring, distillation under reduced pressure, standing for stratification, collecting the lower layer material for suction filtration, After crystallization and drying, 1,4-dimethylpentylamine hydrochloride was obtained.

[0027] A kind of preparati...

Embodiment 1

[0033] A kind of preparation method of 1,4-dimethylamylamine hydrochloride is:

[0034] (1) Amino acylation: Add 11.4 g (0.1 mol) of 5-methyl-2-hexanone into a 500 mL four-neck flask, add 4.6 g (0.1 mol) of formic acid and 7.6 g (0.12 mol) of ammonium formate while stirring. Raise the temperature to 110°C for 3 hours, then raise the temperature to 130°C for 3 hours, and finally keep it at 155°C for 3 hours. Cool to about 40°C and add 40g of water. Stir for 30 minutes, stand to separate the layers, wash the oil layer three times with saturated brine, add anhydrous sodium sulfate to dry overnight, and filter with suction to obtain 11.6g of 1,4-dimethylformyl amylamide oil with a yield of 89.9%, which was directly used in Next reaction.

[0035] (2) Hydrolysis into salt: Add 11.6 g (0.09 mol) of 1,4-dimethylformyl amylamide and 29 g of 36% hydrochloric acid into a 500 mL four-necked flask. The temperature was raised to reflux under stirring for 10 hours. Distill under reduced...

Embodiment 2

[0037] A kind of preparation method of 1,4-dimethylamylamine hydrochloride is:

[0038] (1) Amino acylation: Add 11.4 g (0.1 mol) of 5-methyl-2-hexanone into a 500 mL four-necked flask, and add 6.0 g (0.13 mol) of formic acid and 8.8 g (0.14 mol) of ammonium formate while stirring. Raise the temperature to 115°C for 3 hours, then raise the temperature to 135°C for 3 hours, and finally keep it at 160°C for 3 hours. Cool to about 40°C and add 40g of water. Stir for 30 minutes, stand to separate the layers, wash the oil layer three times with saturated brine, add anhydrous sodium sulfate to dry overnight, and filter with suction to obtain 11.3g of 1,4-dimethylformyl amylamide oil with a yield of 87.6%, which was directly used in Next reaction.

[0039] (2) Hydrolysis into salt: Add 11.3 g (0.088 mol) of 1,4-dimethylformyl amylamide and 33 g of 36% hydrochloric acid into a 500 mL four-necked flask. The temperature was raised to reflux under stirring for 10 hours. Distill under...

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Abstract

The invention discloses a preparation method of 1, 4-dimethyl pentylamine hydrochloride, and relates to the field of organic synthesis preparation chemistry. The preparation method comprises the following steps: by taking 5-methyl-2-hexanone as a raw material, adding a reducing agent formic acid and ammonium formate or formamide while stirring, mixing, heating to 110-115 DEG C, reacting for 3 hours, heating to 130-135 DEG C, reacting for 3 hours, finally heating to 150-160 DEG C, keeping the temperature for 3 hours, cooling, standing for layering, washing, drying, and performing suction filtration to obtain the 1, 4-dimethyl formyl amyl amine; and adding 1, 4-dimethyl formyl pentylamine into hydrochloric acid with the mass concentration of 36%, carrying out heating reflux reaction under stirring, carrying out reduced pressure distillation, performing standing for layering, collecting a lower-layer material, carrying out suction filtration, and carrying out crystallization and drying, thereby obtaining the 1, 4-dimethyl formyl pentylamine. The preparation method of the 1, 4-dimethyl pentylamine hydrochloride provided by the invention is simple, the raw materials are easy to obtain, the process is easy to control, the cost is low, and the preparation method has the characteristics of high yield, clean production, environmental protection and the like, and is suitable for mass production.

Description

technical field [0001] The invention belongs to the field of organic synthesis and preparative chemistry, in particular to a preparation method of 1,4-dimethylamylamine hydrochloride. Background technique [0002] 1,4-Dimethylpentylamine hydrochloride is in the form of hydrolysis of 1,4-dimethylpentylamine into salt by hydrochloric acid. The appearance is white powder with a special smell. It is mainly used as a solvent, alkylation and esterification and polymerization catalysts. This product is mainly used in medicine, nutrition and health products, combined with low-protein diet, prevention and treatment of damage caused by protein metabolism disorders caused by chronic renal insufficiency, the core drug of chronic renal insufficiency and consumptive malnutrition, and other uses In the electroplating industry, the market prospect is very broad. [0003] About synthesizing 1, the literature method of 4-dimethylamylamine hydrochloride is seldom, and the synthetic method of...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C231/08C07C231/10C07C233/03C07C209/62C07C211/07
CPCC07C231/08C07C231/10C07C209/62C07C233/03C07C211/07
Inventor 唐保清付志雄
Owner HUNAN PROVINCE HONGJIANG HUAGUANG BIOTECH
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