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Preparation method of 2-amino-2-methyl-1-propanol

A technology of dimethyl aziridine and methyl, which is applied in the field of preparation of 2-amino-2-methyl-1-propanol, can solve the problems of harsh conditions, easy over-reaction, increased waste pressure, etc., and achieves The effect of mild reaction conditions, high reaction safety, and low environmental pressure

Active Publication Date: 2021-03-09
SUZHOU YACOO SCI CO LTD
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0016] 1) The synthesis of 2-nitropropane as a raw material, the source of raw materials is difficult, the synthesis cost is high, dangerous, the reduction step is easy to overreact, and impurities are generated, which affects the purity of the product
[0017] 2) Using 2-methylalanine methyl ester as raw material is expensive and difficult to obtain, and catalytic hydrogenation requires high temperature and high pressure conditions, and the conditions are relatively harsh
[0018] 3) The route of chlorine gas and isobutylene, both of which are highly toxic and explosive, are limited in use, and the chlorine gas is not transferred to the product, but only acts as an intermediate bridge, and finally becomes waste. First, it causes waste of raw materials, and second, it increases waste pressure, low yield
[0019] 4) With the route of isopropylamine, the cost of catalyst synthesis is very high, the requirements for carbonylation equipment are strict, and the pressure of hydrogen gas required to reduce carbonyl groups is also high, so the cost of industrialization cannot be reduced
[0020] 5) To synthesize 2-amino-2-methyl-1-propanol from 2.2-dimethyl-3-hydroxypropionamide, a strong oxidant hypohalite is used, which will strongly oxidize the hydroxyl in the raw material Aldehyde, and the introduction of impurities, resulting in a serious reduction in product purity

Method used

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  • Preparation method of 2-amino-2-methyl-1-propanol

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preparation example Construction

[0047] The present invention provides a kind of preparation method of 2-amino-2-methyl-1-propanol, its synthetic route is

[0048] Specifically, the preparation method of the 2-amino-2-methyl-1-propanol comprises the following preparation steps:

[0049] S1: Add water into the reaction bottle first, then add dilute sulfuric acid dropwise to the water to make the water slightly acidic, pH=3.5-4, forming a slightly acidic water system;

[0050] S2: Heat the water system obtained in step S1 to 40°C-50°C, and then add 2,2-diethylaziridine and dilute sulfuric acid dropwise at the same time, while maintaining the temperature of 40°C-50°C and slightly acidic conditions 2,2-diethylaziridine was dripped, and reacted at a temperature of 40°C-50°C for 1h, and then distilled under reduced pressure to obtain the reactant;

[0051] S3: dissolving the reactant obtained in step S2 in a solvent, then adding an aqueous sodium hydroxide solution with a mass fraction of 30%, neutralizing to pH...

Embodiment 1

[0057] In a 1L three-neck flask with mechanical stirring, first add 200ml of water, drop a few drops of dilute sulfuric acid to make it slightly acidic (pH=3.5-4), then heat up to 40-50°C, and start adding 80.0 g 2,2-dimethylaziridine and 400ml dilute sulfuric acid aqueous solution, under the conditions of maintaining temperature and slightly acidity, drop 2,2-dimethylaziridine, then continue to react at this temperature 1h, then distill under reduced pressure to remove 80% of the water, add 500ml of ethanol to the obtained system, neutralize with 30% sodium hydroxide to pH = 9.5-10, filter to remove salt, and obtain the filtrate to distill out the ethanol through normal pressure , and then distilled under reduced pressure to obtain the crude product of 2-amino-2-methyl-1-propanol, which was then rectified to obtain 90.0g of 2-amino-2-methyl-1-propanol refined product, with a yield of about 90%, and the chromatographic analysis purity is about 99.5%.

Embodiment 2

[0059] In a 1L three-necked flask with mechanical stirring, first add 200ml of water, drop a few drops of dilute sulfuric acid to make it slightly acidic (pH=3.5-4), then heat up to 40-50°C, and start adding 99.0 g 2,2-dimethylaziridine and 400ml dilute sulfuric acid aqueous solution, under the conditions of maintaining temperature and slightly acidity, drop 2,2-dimethylaziridine, then continue to react at this temperature 1h, then distill under reduced pressure to remove 80% of the water, add 500ml of ethanol to the obtained system, neutralize with 30% sodium hydroxide to pH = 9.5-10, filter to remove salt, and obtain the filtrate to distill out the ethanol through normal pressure , and then distilled under reduced pressure to obtain the crude product of 2-amino-2-methyl-1-propanol, which was then rectified to obtain 112.9g of the refined product of 2-amino-2-methyl-1-propanol, with a yield of about 91.0%, and the chromatographic purity is about 99.4%.

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Abstract

The invention discloses a preparation method of 2-amino-2-methyl-1-propanol, which comprises the following preparation steps: adding 2, 2-dimethyl aziridine into a slightly acidic water system, and reacting at the temperature of below 50 DEG C to obtain a reactant; and neutralizing, roughly distilling and rectifying the reactant to obtain the 2-amino -2-methyl-1-propanol. The method has the advantages of mild reaction conditions, simplicity in operation, easiness in mastering, easiness in treatment of the reaction product, high product purity (the purity is 99.0% or above), high yield (the total yield is 90% or above).

Description

technical field [0001] The invention relates to the technical field of organic synthesis, in particular to a preparation method of 2-amino-2-methyl-1-propanol. Background technique [0002] 2-Amino-2-methyl-1-propanol is a white crystal or colorless viscous liquid, miscible with water and soluble in ethanol. It is a well-known multifunctional additive widely used in coatings, inks, Metalworking fluids, personal care and pharmaceutical intermediates, etc. [0003] The classic synthesis of 2-amino-2-methyl-1-propanol involves: [0004] Using 2-nitropropane as a raw material, the target product is obtained through methylolation, catalytic reduction, rectification and other steps, and its synthetic route is shown in the following formula 1. [0005] [0006] The target product is directly synthesized by catalytic hydrogenation of methyl 2-methylalanine under a pressure of 80-100 atm, and the synthesis route is shown in Formula 2 below. [0007] [0008] At present, ther...

Claims

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Application Information

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IPC IPC(8): C07C213/00C07C213/10C07C215/08
CPCC07C213/00C07C213/10C07C215/08Y02P20/10
Inventor 宋程浩袁永坤
Owner SUZHOU YACOO SCI CO LTD
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