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A kind of preparation method of n-hydroxyphthalimide

A technology of hydroxyphthalimide and phthalic anhydride, applied in the field of preparation of N-hydroxyphthalimide, can solve the problem that the mineralizer ferric oxide is difficult to remove and the reaction time is long , difficult to industrialize and other problems, to achieve the effect of reducing purification energy consumption, reducing toxicity, and reducing solvent toxicity

Active Publication Date: 2017-09-05
NANJING BAOCHUN CHEMICAL INDUSTRY CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The method takes a long time to react, and the operation is complicated, and the mineralizer ferric oxide is difficult to remove, and it is not easy for industrialization

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Put 29.6g of phthalic anhydride and 13.9g of hydroxylamine hydrochloride into 200ml of isopropanol, slowly add 20.2g of triethylamine into the above solution within 30min under stirring at room temperature, and then React for 1.5 hours. After the reaction, distill off isopropanol and triethylamine under reduced pressure, then wash with water and dry at 60°C for 24 hours to obtain 29.4 g of white solid N-hydroxyphthalimide, yield 90.1 %, purity 98.6%.

Embodiment 2

[0024] Put 74.0g of phthalic anhydride and 34.8g of hydroxylamine hydrochloride into 500ml of isopropanol, slowly add 50.5g of triethylamine into the above solution within 30min under stirring at room temperature, and then React for 1 hour. After the reaction, distill off isopropanol and triethylamine under reduced pressure, then wash with water and dry at 60°C for 24 hours to obtain 75.4 g of N-hydroxyphthalimide as a white solid, with a yield of 92.4%. , 98.5% purity.

Embodiment 3

[0026] Put 59.2g of phthalic anhydride and 27.8g of hydroxylamine hydrochloride into 400ml of isopropanol, slowly add 40.4g of triethylamine into the above solution within 30min under stirring at room temperature, and then React for 0.7h. After the reaction is over, distill off isopropanol and triethylamine under reduced pressure, then wash with water and dry at 60°C for 24h to obtain 61.7g of N-hydroxyphthalimide as a white solid, with a yield of 94.6 %, purity 98.7%.

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PUM

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Abstract

The invention relates to a method for preparing N-hydroxyphthalimide. The method includes the following steps: 1, phthalic anhydride and hydroxylamine hydrochloride are added into isopropanol; 2, then triethylamine is added, reacting is carried out for 0.5 h to 1.5 h at the temperature of 70 DEG C to 95 DEG C, reduced pressure distillation is carried out to recycle the isopropanol and the triethylamine, then washing and drying are carried out, and the N-hydroxyphthalimide is obtained. The method has the advantages that the isopropanol is used as new reaction media, and the triethylamine is used as accelerants, so that the toxicity of the solvents is reduced, the reaction safety is improved, the purification energy consumption is reduced, the reaction time is shortened, and the obtained product is high in purity. In addition, compared with inorganic-salt and iron-trioxide purification technology, the purification technology relating to the triethylamine serving as the accelerants is simpler, easy to operate and quite suitable for industrial production.

Description

technical field [0001] The invention relates to the field of chemical industry, in particular to a preparation method of N-hydroxyphthalimide. Background technique [0002] N-Hydroxyphthalimide (NHPI for short) is an important chemical raw material and is widely used in organic synthesis. For example, NHPI can be used as raw material to prepare derivatives of acetaldehyde oxime, RNA peptide conjugates of enzymes as anticancer and antiviral drugs, used as mediator substances in pulp biobleaching process in paper industry, and synthetic nonionic An important intermediate product of the photoacid generator N-hydroxyphthalimide p-toluenesulfonate. In recent years, in the research of biomimetic catalytic system for selective oxidation of hydrocarbons, because it contains >N—OH, it is easy to generate free radicals, so it can be used as an intermediate for transferring electrons in electrochemical oxidation reactions, and can be used for hydrocarbons under mild conditions. Th...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D209/48
CPCC07D209/48
Inventor 陈健张书周健韬杭建荣
Owner NANJING BAOCHUN CHEMICAL INDUSTRY CO LTD