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Preparation method of 2-methyl-1,2-propane diamine

A technology of propylene diamine and methyl, applied in the field of organic synthesis, can solve the problems of difficult industrialization yield, unfavorable industrialization, unstable raw materials, etc., and achieves the effects of high reaction yield, easy industrialization, and low cost

Inactive Publication Date: 2013-03-20
张家港市大伟助剂有限公司
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  • Abstract
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Problems solved by technology

[0003] Although 2-methyl-1,2-propanediamine is widely used, its preparation method has disadvantages such as unstable raw materials, long preparation time, many side reactions, difficult industrialization and low yield, which is not conducive to industrialization

Method used

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  • Preparation method of 2-methyl-1,2-propane diamine

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Embodiment

[0023] 1) Preparation of α-aminoisobutyronitrile (I)

[0024] Add 68g of ammonia water and 32.1g (0.6mol) of ammonium chloride into the reactor, stir to dissolve, add 59.5g (3.5mol) of liquid ammonia into the reactor at 0-5°C, and drop 85g (1mol) of acetone cyanohydrin at the same time, 28 React at ~30°C for 3 hours, GC detects that the raw materials have reacted completely, and the reaction is completed, add tetrahydrofuran to separate the organic layer, extract the water layer with tetrahydrofuran, combine the organic layers, dry over anhydrous sodium sulfate, filter, and collect the 60°C / 267kPa fraction by vacuum distillation of the filtrate , to obtain α-aminoisobutyronitrile (I) (colorless liquid 76.7g, yield 86.9%, content 99.9% (determined by GC area normalization method));

[0025] 2) Preparation of α-acetylaminoisobutyronitrile (II)

[0026] Add 76.5g (0.75mol) of acetic anhydride to the reactor, cool down to 0-5°C, add 25.2g (0.3mol) of α-aminoisobutyronitrile (I) d...

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Abstract

The invention discloses a preparation method of 2-methyl-1,2-propane diamine. The method comprises the following preparation steps of: 1) preparing alpha-amino isobutyronitrile (I); 2) preparing alpha-acetamido isobutyronitrile (II); 3) preparing 2,4,4-trimethyl-2-imidazoline (III); and 4) preparing 2-methyl-1,2-propane diamine (IV). The preparation method disclosed by the invention has the advantages of stable raw materials, low cost, mild reaction conditions and high reaction yield and is easy to industrialize. The solvent in the reaction process can be recycled by distilling.

Description

technical field [0001] The invention belongs to the field of organic synthesis, and in particular relates to a preparation method of 2-methyl-1,2-propanediamine. Background technique [0002] 2-Methyl-1,2-propanediamine is an important intermediate for the preparation of a new generation of antimalarial drug OZ277 (Arterolane) [H]. 02277 overcomes the resistance of pathogens to traditional antimalarial drugs, and is effective when taken orally, has low toxicity, is easy to absorb, has a long duration of drug effect, and has a broad market prospect. The corresponding intermediate 2-methyl-1,2-propanediamine The demand is also increasing year by year. In addition, 2-methyl-1,2-propylenediamine is also an ideal raw material for preparing batteries, metal chelating agents, coolants, gel inhibitors, polyamides, etc. [0003] Although 2-methyl-1,2-propanediamine is widely used, its preparation method has disadvantages such as unstable raw materials, long preparation time, many s...

Claims

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Application Information

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IPC IPC(8): C07C211/11C07C209/62
Inventor 龚卫良黄德周
Owner 张家港市大伟助剂有限公司
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