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Method for preparing N-butylphthalimide

A technology of butylphthalimide and n-butylamine, applied in the chemical field, can solve the problems of high production cost, complicated operation, large amount of three wastes and the like, and achieve the effects of high production efficiency and simple process

Inactive Publication Date: 2012-02-08
山东昌邑灶户盐化有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] N-butyl phthalimide is an intermediate used to prepare dyes, medicines, spices, etc. The current synthesis method mainly uses phthalic anhydride as raw material, and first reacts with urea or ammonia water to form phthalimide. Under the action of acid-binding agent potassium carbonate, N-substitution reaction occurs with bromobutane to obtain N-butylphthalimide. This method is divided into two steps, with long flow process, complicated operation, and large amount of three wastes. high production cost

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] In the reaction flask, add 10 g of water successively, 15.8 g (0.21 mol) of n-butylamine with a mass content of 97%, 29.9 g (0.2 mol) of phthalic anhydride and 1.39 g of tetrabutylammonium chloride with a mass content of 99%, and open Stir, heat until the phthalic anhydride is completely dissolved, continue heating to reflux, react at 135°C for 5 hours, then cool down to 60°C, pour the reaction solution into a separatory funnel, let it stand, and separate it when it cools down to 40°C to obtain light Yellow oily liquid, the water phase is used as the mother liquor, and the oily liquid is washed twice with warm water at 40°C, cooled and solidified to obtain 36.8 g of N-butylphthalimide, calculated as phthalic anhydride, with a yield of 90.6% and a melting point of 29~ 31°C.

Embodiment 2

[0019] In the reaction flask, add 10 g of water, 15.1 g (0.2 mol) of n-butylamine with a mass content of 97%, 29.9 g (0.2 mol) of phthalic anhydride with a mass content of 99% and 0.03 g of benzyltrimethylammonium chloride , start stirring, heat until the phthalic anhydride is completely dissolved, continue heating to reflux, react at 100°C for 2 hours, then cool down to 55°C, pour the reaction solution into a separatory funnel, let it stand, and separate it when it cools down to 35°C to obtain Pale yellow oily liquid, the water phase was recycled as mother liquor, the oily liquid was washed three times with warm water at 35°C, cooled and solidified to obtain 27.2 g of N-butylphthalimide, calculated as phthalic anhydride, with a yield of 67% and a melting point of 29 ~31°C.

Embodiment 3

[0021] Adding mass content successively in reaction flask is 97% n-butylamine 20.54g (0.26 mol), mass content is 99% phthalic anhydride 29.9 g (0.2 mol) and 4.95g phenyl trimethyl ammonium chloride, start stirring, Heat until the phthalic anhydride is fully dissolved, continue heating to reflux, and react at 160°C for 20 hours, then cool down to below 100°C, add 10g of water, continue to cool down to 65°C, pour the reaction solution into a separatory funnel, let it stand, and cool down to Separate at 45°C to obtain a light yellow oily liquid, wash the oily liquid once with warm water at 45°C, and cool to solidify to obtain 39.3 g of N-butylphthalimide, calculated as phthalic anhydride, with a yield of 96.7% and a melting point of 29 ~31°C.

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Abstract

The invention discloses a method for preparing N-butylphthalimide, which comprises the following steps of: (1) a charging reaction step: adopting phthalic anhydride and n-butylamine as raw materials, taking water as solvent, and carrying out reflux reaction for 0.5-20 hours at the temperature of 100-160 DEG C under the action of phase transfer catalyst to obtain slight yellow turbidliquid; and (2) a cooling separation step: cooling to 55-65 DEG C after reaction is finished, static placing and layering, and separating to obtain slight yellow oilyliquid, i.e. the N-butylphthalimide when the temperature goes down to 35-45 DEG C. The method disclosed by the invention has simple process, is environmentally-friendly and non-toxic, and has high production efficiency.

Description

technical field [0001] The invention relates to the technical field of chemical industry, in particular to a method for preparing N-butylphthalimide. Background technique [0002] N-butyl phthalimide is an intermediate used to prepare dyes, medicines, spices, etc. The current synthesis method mainly uses phthalic anhydride as raw material, and first reacts with urea or ammonia water to form phthalimide. Under the action of acid-binding agent potassium carbonate, N-substitution reaction occurs with bromobutane to obtain N-butylphthalimide. This method is divided into two steps, with long flow process, complicated operation, and large amount of three wastes. Production costs are high. Contents of the invention [0003] The technical problem to be solved by the present invention is to provide a method for preparing N-butylphthalimide with simple process, environmental protection and non-toxicity. [0004] For solving the problems of the technologies described above, technic...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D209/48
Inventor 付忠东高建伟解德水万克玲梁足培
Owner 山东昌邑灶户盐化有限公司
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