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Preparation method of 1, 3-dimethyl-pentylaminehydrochloride

A technology of dimethylpentylamine hydrochloride and methyl group, which is applied in the field of organic synthesis and preparation chemistry, can solve the problems of high industrialization cost, poor product purity, and many process steps, and achieves low production cost, simple operation and controllability. strong effect

Active Publication Date: 2013-12-25
上海倍殊生物科技有限公司
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Problems solved by technology

All reported routes are subject to the synthesis and cost of 4-methyl-2-hexanone, and the purity of the product obtained by using the 4-methyl-2-hexanone route is relatively poor, the process steps are many and the operation is complicated, and industrialization high cost

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  • Preparation method of 1, 3-dimethyl-pentylaminehydrochloride

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preparation example Construction

[0023] A kind of preparation method of 1,3-dimethylamylamine hydrochloride, the reaction process schematic diagram of its preparation method is as figure 1 shown, namely

[0024] Firstly, using 2-methylbutyraldehyde as the starting material, in toluene solvent, the ethylenediamine and acetic acid composite catalyst are used to catalyze the condensation reaction of 2-methylbutyraldehyde and nitroethane to prepare nitroolefin compounds;

[0025] Then, the resulting nitroalkene compound is subjected to an alkene reduction reaction by potassium borohydride or sodium borohydride in a mixed solvent composed of toluene and water under the condition of a phase transfer catalyst to obtain 4-methyl 2-nitro Hexane;

[0026] Then, the obtained 4-methyl 2-nitrohexane, in an alcohol solvent, is hydrogenated and reduced to an amino group by palladium carbon, and then salified by hydrochloric acid to obtain 1,3-dimethylpentylamine hydrochloride Crude salt;

[0027] Finally, the obtained cr...

Embodiment 1

[0029] A kind of preparation method of 1,3-dimethylamylamine hydrochloride, specifically comprises the steps:

[0030] (1) In a 500mL reaction bottle, add 165g of solvent 1, add 3.4g of ethylenediamine, slowly add 6.8g of acetic acid dropwise under stirring, then dropwise add 70g of 2-methylbutyraldehyde, and then slowly dropwise add nitro Ethane 67g, control the temperature at 84-88°C to reflux with water to react for 8-10h, after the reaction is completed, cool to below 35°C, add 50ml of water, stir for static separation, remove the water layer, and the obtained toluene-containing organic The phase is the crude product of nitroolefin compound;

[0031] Described solvent 1 is toluene;

[0032] In the process of condensation and dehydration of 2-methylbutyraldehyde and nitroethane in the above steps, calculated by molar ratio, that is, 2-methylbutanal: nitroethane: composite catalyst is 1:1.0:0.1;

[0033] (2) Pour the crude nitroolefin compound obtained in step (1) into a 5...

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Abstract

The invention discloses a preparation method of 1, 3-dimethyl-pentylaminehydrochloride. The preparation method comprises the following steps: performing condensation and dehydration on 2-methylbutyraldehyde used a starting material and nitroethane under the catalyzing of an acetic acid / ethylenediamine composite catalyst in a methylbenzene solvent to obtain a nitroolefin compound; reducing through potassium borohydride or sodium borohydride; then reducing through palladium carbon and acidizing through hydrochloric acid to obtain 1, 3-dimethyl-pentylaminehydrochloride. The preparation method of 1, 3-dimethyl-pentylaminehydrochloride has the advantages that the raw materials are simple and easy to obtain; the reaction condition is mild; the total yield is high; the industrial production can be performed well.

Description

technical field [0001] The invention relates to a preparation method of 1,3-dimethylamylamine hydrochloride, which belongs to the field of organic synthesis and preparation chemistry. Background technique [0002] Dimethylpentylamine hydrochloride, also known as 1,3-dimethylpentylamine hydrochloride, is the hydrochloride form of 1,3-dimethylpentylamine. Appearance is white crystalline powder. There is a specific smell. An adrenaline-mimetic drug first launched by the American Lilly Company under the trade name of Forthane. At the same time, the product is also used as a functional additive for pharmaceutical intermediates, catalysts and health products. The literature introduces that the synthetic method of 1,3-dimethylpentylamine hydrochloride mainly focuses on the use of 4-methyl-2-hexanone route, such as a) catalytic hydrogenation after condensation with hydroxylamine sulfate (or metal sodium reduction ); b) under the condition of catalytic hydrogenation, condense it...

Claims

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Application Information

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IPC IPC(8): C07C211/07C07C209/34C07C209/00
Inventor 刘传祥刘利刚丁文吴智影王宇凯王永
Owner 上海倍殊生物科技有限公司
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