Method for preparing 2-amino-2-methyl-1-propanol

A technology of methylpropionitrile and methyl, which is applied in the field of preparing 2-amino-2-methyl-1-propanol, can solve the problems of limited source of raw materials, complicated process, complicated preparation steps, etc., and achieves obvious cost advantages, The reaction process is simple and the effect of product purification

Active Publication Date: 2017-09-05
WANHUA CHEM GRP CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This preparation method also has its disadvantages, that is, there are many kinds of reaction raw materials, the preparation steps are complicated, and the yield is low.
[0007] The existing method for preparing 2-amino-2-methyl-1-propanol has problems such as limited sources of raw materials, explosive raw materials and intermediates, complicated process, complicated post-treatment, and low yield.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] Weigh 117g of sodium cyanide and grind it finely, add it to 120g of water at room temperature, and stir until the sodium cyanide is completely dissolved. Weigh 157g of 2-chloropropane and 160g of ethanol and mix them, then slowly drop them into the aqueous sodium cyanide solution, and after the dropwise addition, raise the temperature to 95°C for 4 hours. Cool down after the end of the reaction, filter and remove the precipitated sodium chloride solid, wash the filtrate twice with about 20g ethanol, combine the filtrate and carry out distillation to remove ethanol and water, filter again to remove sodium cyanide and sodium chloride precipitation, obtain 141g thick 2-formazan propionitrile, the purity is about 87.9%, and the target product yield of this step is about 90%.

[0036] Crude 2-methylpropionitrile was mixed with 182g 37wt% formaldehyde aqueous solution, and 21g 30wt% trimethylamine aqueous solution was added dropwise under stirring, and reacted at 45°C for 1.5...

Embodiment 2

[0041] Weigh 98g of sodium cyanide and grind it finely, add it into 53g of water at room temperature, and stir until the sodium cyanide is completely dissolved. Weigh 157g of 2-chloropropane and 85g of ethanol and mix them, then slowly drop them into the aqueous sodium cyanide solution, and after the dropwise addition, raise the temperature to 80°C for 8 hours of reaction. Cool down after the end of the reaction, filter and remove the precipitated sodium chloride solid, wash the filtrate twice with about 20g of ethanol, combine the filtrate and carry out distillation to remove ethanol and water, filter again to remove sodium cyanide and sodium chloride precipitation, obtain 142g thick 2-formazan propionitrile, the purity is about 82.4%, and the target product yield of this step is about 84.8%.

[0042] Crude 2-methylpropionitrile was mixed with 172g of 37% formaldehyde aqueous solution, 30g of 30wt% trimethylamine aqueous solution was added dropwise under stirring, and reacted...

Embodiment 3

[0047] Weigh 127g of sodium cyanide and grind it finely, add it into 237g of water at room temperature, and stir until the sodium cyanide is completely dissolved. Weigh 157g of 2-chloropropane and 290g of ethanol and mix them, then slowly drop them into the aqueous sodium cyanide solution, and after the dropwise addition, raise the temperature to 105°C for 3 hours of reaction. Cool down after reaction finishes, filter and remove the sodium chloride solid that separates out, wash filtrate twice with about 20g ethanol, combine filtrate and carry out distillation and remove ethanol and water, filter again and remove sodium cyanide and sodium chloride precipitation, obtain 139.4g thick 2- Methylpropionitrile has a purity of about 87.1%, and the yield of the target product in this step is about 88%.

[0048] Crude 2-methylpropionitrile was mixed with 150g of 37wt% formaldehyde aqueous solution, 5.3g of triethylamine was added dropwise under stirring, and reacted at 60°C for 50min. ...

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PUM

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Abstract

The invention relates to a method for preparing 2-amino-2-methyl-1-propanol. The method comprises the following steps: 1) enabling 2-chloropropane and sodium cyanide to react to generate 2-methyl propionitrile; 2) performing aldol condensation reaction on the 2-methyl propionitrile and formaldehyde so as to generate 2,2-dimethyl-3-hydroxy propionitrile; 3) performing hydrolysis reaction on 2,2-dimethyl-3-hydroxy propionitrile so as to generate 2,2-dimethyl-3-hydroxy propanamide; and 4) performing Hofmann degradation on the 2,2-dimethyl-3-hydroxy propanamide, thereby obtaining 2-amino-2-methyl-1-propanol. The method is cheap and easy in obtaining of raw materials of different steps, simple in reaction process, free of hash reaction condition, remarkable in cost advantage, high in yield, low in pollution and easy in product purification.

Description

technical field [0001] The invention relates to a method for preparing 2-amino-2-methyl-1-propanol, belonging to the field of organic synthesis. Background technique [0002] 2-Amino-2-methyl-1-propanol is white crystal or colorless viscous liquid, miscible with water and soluble in ethanol. It is a well-known multifunctional additive widely used in paint ink, metal In industries such as processing fluids, personal care and pharmaceutical intermediates. As a primary amine, 2-amino-2-methyl-1-propanol has a high pH value due to its high pKa value. At the same time, because it is an organic base, it is relatively soft and compatible with various emulsions. Good compatibility, less impact on other properties of the product. Compared with other organic bases such as ammonia, trimethylamine and triethylamine, 2-amino-2-methyl-1-propanol has good stability, is not easy to yellow, and has low toxicity and is not volatile, which can reduce the system Odor, reduce corrosion and fl...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C213/02C07C215/08
CPCC07C213/02C07C231/06C07C253/14C07C253/30C07C215/08C07C235/06C07C255/12C07C255/03
Inventor 王鹏何光文崔乾丛鑫黎源
Owner WANHUA CHEM GRP CO LTD
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