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Synthetic method of oxo-bis(n-methylphthalimide)

A technology of methylphthalimide and phthalimide, which is applied in the field of synthesis of oxo-bis(N-methylphthalimide), can solve the problem of low yield , environmental pollution, increased production costs and other issues, to achieve the effect of simple reaction operation, high process safety and low production cost

Active Publication Date: 2021-06-18
CHANGZHOU SUNLIGHT PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] (1) Using conventional basic catalysts and phase transfer catalysts, the yield is low
[0009] (2) It is necessary to use a relatively expensive self-made catalyst to obtain the ideal yield, which will not only cause a significant increase in production costs, but also the self-made catalyst is not easy to obtain, and is not suitable for industrialized large-scale production
[0010] (3) Since the phase transfer catalyst cannot be reused, it can only be directly turned into solid waste, causing great environmental pollution
[0011] (4) The purity of the product is not ideal, generally it can only reach 95%~97%

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1）

[0030] The synthetic method of the oxo-bis(N-methylphthalimide) of the present embodiment is specifically as follows:

[0031] Add 20.6g of 4-nitro-N-methyl-phthalimide (0.1mol) and 17.7g of 4-hydroxy-N-methyl-phthalimide to the reaction kettle in sequence (0.1mol), 20.7g of potassium carbonate (0.15mol), 20mL of toluene and 40mL of DMF, stirred and heated to reflux, and the reaction was complete.

[0032] After the reaction, the reaction system was lowered to room temperature (20±5°C), then added to water with stirring, filtered, and the filter cake was recrystallized with 60mL of ethanol to obtain 30.3g of oxo-bis(N-methylphthalate formimide), the yield was 90.2%, and the purity was 99.6% (HPLC).

Embodiment 2～ Embodiment 5）

[0034] The synthesis method of each embodiment is basically the same as that of Example 1, and the differences are shown in Table 1.

[0035] Table 1

[0036] Example 1 Example 2 Example 3 Example 4 Example 5 potassium carbonate 20.7g (0.15mol) 20.7g (0.15mol) 20.7g (0.15mol) 13.8g (0.10mol) 27.6g (0.2mol) Toluene 20mL 20mL 20mL 20mL 20mL DMF 40mL 30mL 50mL 40mL 40mL product weight 30.3g 29.5g 28.6g 29.4g 30.5g yield 90.2% 87.8% 85.1% 87.5% 90.8% purity 99.6% 99.6% 99.5% 99.6% 99.7%

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Abstract

The invention discloses a synthetic method of oxo-bis(N-methylphthalimide), which is composed of 4-nitro-N-methyl-phthalimide and 4- Hydroxyl-N-methyl-phthalimide is obtained by nucleophilic substitution reaction in the presence of a basic catalyst in a mixed solvent. The mixed solvent is composed of a benzene solvent and an aprotic polar solvent in a volume ratio of 1:1˜1:5. The method of the present invention does not need to use expensive self-made catalysts, and does not need to use phase transfer catalysts that pollute the environment. It only needs to use conventional basic catalysts to react in mixed solvents. The reaction is simple in operation, high in process safety, and low in production costs. Lower, less environmental pollution, especially higher reaction yield, high product purity, which is suitable for industrial production.

Description

technical field [0001] The invention belongs to the technical field of fine chemicals, and in particular relates to a synthesis method of oxo-bis(N-methylphthalimide). Background technique [0002] 3,3',4,4'-Diphenyl ether tetracarboxylic dianhydride (hereinafter referred to as ODPA) is a new type of special engineering plastics polyimide, polyetherimide, polyesterimide, polyamideimide, polyimide One of the important monomers of high temperature resistant resins such as maleimide and polyaramid. ODPA polyimide has outstanding mechanical properties, electrical properties, and radiation resistance, and can be used for a long time in the range of -269 to 250 °C. Since ODPA introduces flexible ether bonds into the main chain structure of polyimide, which greatly reduces the softening temperature, it belongs to thermoplastic polyimide and has good processing performance. It has been widely used in my country's aerospace and other high-tech fields. [0003] Oxo-bis(N-methylphtha...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D209/48
CPCC07D209/48
Inventor 胡国宜胡锦平郑奎李喜龙奚小金
Owner CHANGZHOU SUNLIGHT PHARMA