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N-methylphthalimide preparation process

A technology of methyl phthalimide and preparation process is applied in the field of preparation of N-methyl phthalimide and achieves the effects of good handling, low cost and complete reaction

Inactive Publication Date: 2006-11-22
诸亚明 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0013] The purpose of this invention is to provide a kind of preparation technology of new N-methylphthalimide, the technical problem that needs to be solved is: simplify preparation process flow, improve reaction speed, improve yield and the purity of product, Eliminate environmental pollution

Method used

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  • N-methylphthalimide preparation process
  • N-methylphthalimide preparation process
  • N-methylphthalimide preparation process

Examples

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Effect test

Embodiment 1

[0020] Example 1: Put 200 grams of phthalic anhydride into a 250ml four-necked glass reaction bottle, heat it at 140±10°C under the protection of helium, feed 46 grams of methylamine gas, react for 4 hours, and add 500 grams of dioxane dropwise while hot Crystals were precipitated in the ring solvent container, filtered, and dried to obtain 206.7 g of white crystals, with a yield of 95% and a purity of 99.4%.

Embodiment 2

[0021] Example 2: Put 400 grams of phthalic anhydride into a 500ml four-necked glass reaction bottle and heat it under the protection of nitrogen at 180±10°C. Stir and feed 90 grams of methylamine gas to react for 2.5 hours. Add 900 grams of dimethyl dimethicone dropwise while hot. White crystals were precipitated in the container of formamide solvent, filtered and dried to obtain 413 g of white crystals with a yield of 95% and a purity of 99.6%.

Embodiment 3

[0022] Example 3: Put 800 grams of phthalic anhydride into a 1000ml four-necked glass reaction bottle and heat it under the protection of nitrogen at 220±10°C. Stir and feed 180 grams of methylamine gas to react for 2 hours, then add dropwise to a container with 1800 grams of ethanol solvent while hot White crystals were precipitated in the mixture, filtered, and dried to obtain 844 grams of white crystals, with a yield of 97% and a purity of 99.7%.

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Abstract

The invention relates to a preparation method of N-methylphthalimide. The invention solves the defects of complex technological process, heavy solvent recovery workload, environmental pollution, low product purity, low yield and the like existing in the existing N-methylphthalimide preparation method. The preparation technology of N-methylphthalimide is characterized in that: use phthalic anhydride as raw material, under the condition of no solvent and inert gas, feed methylamine gas to react, after the reaction finishes, add dropwise water-soluble solvent, Precipitate N-methylphthalimide crystals, shake dry and filter to obtain the finished product. The obtained N-methylphthalimide is an intermediate for synthesizing medicines, dyes and insecticides and is used for synthesizing chemiluminescent immunoassay reagents.

Description

1. Technical field [0001] The invention relates to a preparation method of N-methylphthalimide. 2. Background technology: [0002] The English name of N-methylphthalimide is N-Methyl-o-phthalimide, referred to as NMP, NMP is an important chemical raw material, because it contains (N-methyl) H is very active and contains aromatics Structure, can be used as an intermediate in the synthesis of drugs, dyes and pesticides. In recent years, the application of NMP in the synthesis of chemiluminescent immunoassay reagents will have potential application prospects. Therefore, the research on the synthesis method of this compound is becoming more and more important. [0003] Regarding the synthesis of NMP, domestic and foreign literature reports, the synthesis method mainly has A, B and big categories. Type A is prepared by reacting phthalimide in absolute ethanol and potassium hydroxide to produce potassium salt, and then carrying out alkylation reaction of potassium salt and dimet...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D209/48
Inventor 瞿渊义
Owner 诸亚明