Method for synthesizing N-hydroxy phthalimide with solid-phase process
A hydroxyphthalimide, solid-phase synthesis technology, applied in the direction of organic chemistry and the like, can solve the problems of high energy consumption, waste water pollution, low yield and the like, achieve low energy consumption, improve yield and purity, high yield effect
Inactive Publication Date: 2010-09-29
JIANGSU CHENPAI PHARM GRP CO LTD
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Problems solved by technology
[0004] The above-mentioned synthetic methods all adopt a conventional liquid phase reaction system, which has the disadvantages of waste water pollution, high energy consumption, and low yield.
Method used
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Experimental program
Comparison scheme
Effect test
Embodiment 1
[0021] Take 37.4g of phthalic anhydride and 37.4mg of sodium chloride, mix them, and grind them for 4.5 hours under the protection of nitrogen. Then add 17.7 g of hydroxylamine hydrochloride and 17.7 mg of ferric oxide, grind at 90° C. for 4 hours under nitrogen protection, wash with water, and dry to obtain 38.3 g of white solid with a purity of 98.5%.
Embodiment 2
[0023] Take 74.0 g of phthalic anhydride and 74 mg of sodium chloride, mix them, and grind them for 4.5 hours under the protection of nitrogen. Then add 35 g of hydroxylamine hydrochloride and 35 mg of ferric oxide, grind at 95° C. for 5 hours under nitrogen protection, wash with water, and dry to obtain 77.0 g of white solid with a purity of 98.0%.
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The invention discloses a method for synthesizing N-hydroxy phthalimide with the solid-phase process by grinding the raw materials of phthalic anhydride and hydroxylamine hydrochloride and the mineralizer of sodium chloride and ferric oxide under the protection of nitrogen. The method for synthesizing N-hydroxy phthalimide with the solid-phase process ensures the thorough reaction, high yield, low energy consumption and less pollution and is suitable for industrial production, thereby being a promising preparation method.
Description
field of invention [0001] The invention relates to a method for synthesizing a compound by a solid-phase method, in particular to a solid-phase synthesis method for the compound N-hydroxyphthalimide (abbreviated as HP), and belongs to the technical field of chemical synthesis. Background technique [0002] HP is an important chemical raw material, which can be used as an intermediate in the synthesis of drugs and pesticides. Because it contains N-OH, it is easy to generate free radicals, so it can also be used as an intermediate mediator for transferring electrons in electrochemical oxidation reactions. In recent years, the application of HP as an electron transporter in electrochemical reactions and as a mediator substance in pulp biobleaching process will have potential application prospects, so the research on the synthesis method of this compound is becoming increasingly important. [0003] Regarding the synthesis of HP, it is used as an intermediate product in the Chine...
Claims
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IPC IPC(8): C07D209/48
Inventor 李瑞菊陈子雷王丰恩方丽平董崭
Owner JIANGSU CHENPAI PHARM GRP CO LTD