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Method for synthesizing 2- amino-2-methyl-1-propanol from isopropylamine

A technology of isopropylamine and amino group, applied in the field of synthesizing 2-amino-2-methyl-1-propanol from isopropylamine, can solve the problems of limited raw material sources, complicated preparation steps, complicated post-processing, etc., and achieves wide raw material sources. , mild conditions, easy separation effect

Active Publication Date: 2016-03-23
JIUJIANG TINCI ADVANCED MATERIALS CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

This preparation method also has its disadvantages, that is, there are many types of reaction raw materials, the preparation steps are complicated, and the yield is low, and the yield is 50-70%.
[0006] 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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  • Method for synthesizing 2- amino-2-methyl-1-propanol from isopropylamine
  • Method for synthesizing 2- amino-2-methyl-1-propanol from isopropylamine
  • Method for synthesizing 2- amino-2-methyl-1-propanol from isopropylamine

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Experimental program
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Effect test

Embodiment 1

[0044] Take 300g of diphenyl ether, 30g (0.51mol) of isopropylamine, 11.25g (50mmol) of palladium acetate and 65.5g (250mmol) of triphenylphosphine, and add them to a 1000mL autoclave in turn, and feed the synthesis gas into the autoclave To a pressure of 3MPa, the synthesis gas is H with a molar ratio of 1:1 2 Mixed gas with CO, start stirring and raise the temperature to 140°C. When the temperature rose to 140°C, the pressure was supplemented with syngas to 8MPa to start the timing reaction. During the reaction process, the syngas pressure is supplemented intermittently to maintain the reaction pressure at 7-8 MPa. Gas chromatographic tracking found that 6h isopropylamine was no longer converted, and this time the temperature was lowered to stop the reaction.

[0045] The reaction solution was taken out, distilled under reduced pressure at 2.5kPa, and the fraction between 68°C and 72°C was collected to obtain 40.85g of pure 2-amino-2-methyl-1-propanol, with a yield of 90%....

Embodiment 2

[0050] Get the distillation still raffinate in Example 1 and join in the 1000mL autoclave, then add isopropylamine 30g (0.51mol), pass the syngas into the autoclave until the pressure is 3MPa, the syngas molar ratio is 1:1 H 2 Mixed gas with CO, start stirring and raise the temperature to 140°C. When the temperature rose to 140°C, the pressure was supplemented with syngas to 8MPa to start the timing reaction. During the reaction process, the syngas pressure is supplemented intermittently to maintain the reaction pressure at 7-8 MPa. The reaction was finished after 6h. The conversion rate of isopropylamine and the yield of 2-amino-2-methyl-1-propanol were calculated from the reaction liquid by gas chromatography external standard method. Record it as the first application. After repeated application by analogy, conversion rate and yield are obtained as shown in Table 1.

[0051] Table 1

[0052] Apply times

[0053] 12

Embodiment 3

[0054] Embodiment 3 (solvent 100, catalyst 1mol%, ligand 2, temperature 100, pressure 1)

[0055] Take 300g of diphenyl ether, 3g (51mmol) of isopropylamine, 0.13g (0.5mmol) of palladium acetate and 0.262g (1mmol) of triphenylphosphine, and add them to a 1000mL autoclave in turn, and feed the synthesis gas into the autoclave To a pressure of 0.5MPa, the synthesis gas is H with a molar ratio of 1:1 2 Mixed gas with CO, start stirring and raise the temperature to 100°C. When the temperature rose to 100°C, the pressure was supplemented with syngas to 1 MPa to start the timing reaction. During the reaction process, the synthesis gas pressure is supplemented intermittently to maintain the reaction pressure at 0.8-1 MPa. Gas chromatography followed until the isopropylamine no longer reacted. The conversion rate of isopropylamine was 17%, and the yield of 2-amino-2-methyl-1-propanol was 15%.

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Abstract

The present invention relates to a method for synthesizing 2-amino-2-methyl-1-propanol from isopropylamine. The isopropylamine reacts with syngas in the presence of a metal catalyst, a ligand and a solvent at the temperature of 100-200 DEG C and at the pressure of 0.8-20 MPa so as to obtain the 2-amino-2-methyl-1-propanol. According to the method, the reactive strategies of metal catalyst in situ preparation, amidogen alpha-position C-H bond activation and hydrogenation one-pot procedure are adopted, the method is wide in raw material resources, simple in steps, mild in condition and easy in separation, and the yield can reach 93%, so that the method is suitable for industrial production.

Description

technical field [0001] The invention relates to a method for synthesizing 2-amino-2-methyl-1-propanol from isopropylamine. 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 industries such as coating inks, metalworking fluids, personal care and pharmaceutical intermediates. [0003] In the existing industrialization technology, the 2-nitropropane route represented by DOW Chemical Company, such as US8674139, uses formaldehyde as a raw material to obtain 2-amino-2-methyl-1-propanol product through condensation and hydrogenation . This route uses the propane nitration process to produce 2-nitropropane, which has low nitration selectivity and is prone to explosion. [0004] Chinese patent CN1810767 discloses a similar preparation method, which differs from the above-mentioned route in the source of 2-nitro-2-methyl-1-prop...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C213/00C07C215/08
CPCC07C213/00C07C215/08
Inventor 赵经纬信勇
Owner JIUJIANG TINCI ADVANCED MATERIALS CO LTD
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