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Preparation method of N-benzyl phthalimide

A technology of benzyl phthalimide and phthalic acid, which is applied in the field of preparation of N-benzyl phthalimide, can solve the problem that the reaction raw materials are not easy to mix uniformly, heat cannot be removed quickly, It is unfavorable for industrialized production and other issues, and achieves the effect of being conducive to environmental protection, simple post-processing method, and conducive to industrialized production

Active Publication Date: 2021-02-26
内蒙古源宏精细化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

In the first two methods, the reaction conditions are harsh, and accompanied by the sublimation of phthalic anhydride and environmental pollution.
The urea method is a more commonly used synthetic method in industry recently, but the reaction raw materials are not easy to mix uniformly, and the heat released by the reaction cannot be removed quickly, which is not conducive to industrial production

Method used

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  • Preparation method of N-benzyl phthalimide
  • Preparation method of N-benzyl phthalimide
  • Preparation method of N-benzyl phthalimide

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Preparation of triethylamine / trinitromethane eutectic catalyst:

[0025] Add 100mL of ethanol to the reactor, then add 20.2g of triethylamine and 30.2g of trinitromethane, stir and mix evenly, then stir at normal temperature and pressure for 2 hours, and distill off the solvent ethanol under reduced pressure to obtain 48.4g of yellow liquid , the yield was 96%.

Embodiment 2

[0027] Preparation of N-benzylphthalimide:

[0028] Add 100mL N,N-dimethylformamide (DMF) into the reactor, then add phthalic acid (16.3g, 0.1mol), stir and mix at room temperature, then add benzylamine (16.1g, 0.15mol) and triethylamine / trinitromethane eutectic catalyst (3g), the addition was completed, and the reaction was continued for 3 hours at room temperature and normal pressure. After the reaction, add 100mL of toluene, cool to 0-5°C, filter to obtain the target compound N-benzylphthalimide, then recrystallize with ethanol as a solvent, collect the solid by filtration, and dry it in vacuum to obtain Refined N-benzylphthalimide white needle-like solid 20.9g, its yield is 88%, and adopts HPLC area normalization method to measure its purity to be 99.8%.

Embodiment 3

[0030] Preparation of N-benzylphthalimide:

[0031] Add 100mL N,N-dimethylformamide (DMF) into the reactor, then add phthalic acid (16.5g, 0.15mol), stir and mix at room temperature, then add benzylamine (21.5g , 0.2mol) and triethylamine / trinitromethane eutectic catalyst (2g), the addition was completed, and the reaction was continued for 2 hours at room temperature and normal pressure. After the reaction, add 100mL of toluene, cool to 0-5°C, filter to obtain the target compound N-benzylphthalimide, then recrystallize with ethanol as a solvent, collect the solid by filtration, and dry it in vacuum to obtain Refined N-benzylphthalimide white needle-like solid 20.1g, its yield is 85%, and its purity measured by HPLC area normalization method is 99.8%.

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Abstract

The invention provides a preparation method of N-benzyl phthalimide, which comprises the steps of by using phthalic acid and benzylamine as raw materials, N,N-dimethyl formamide or dimethylacetamide as a solvent and triethylamine / trinitromethane eutectic as a catalyst, reacting at normal temperature and normal pressure; and after the reaction is finished, supplementing a proper amount of methylbenzene, cooling to the temperature of 0-5 DEG C, and filtering to obtain the target compound N-benzyl phthalimide. The preparation method disclosed by the invention is simple in reaction step process, high in yield, high in product purity, mild in condition and easy for industrial production.

Description

technical field [0001] The invention belongs to the field of organic chemistry, and in particular relates to a preparation method of N-benzylphthalimide. Background technique [0002] N-benzylphthalimide, also known as N-benzyl imide, is a white crystal and can be used as a raw material for a variety of fine chemicals. It is an important intermediate for the synthesis of aliphatic primary amines and α-amino acids. It can be used as an intermediate of medicine and pesticide, and is widely used in medicine, pesticide, rubber, dyestuff and other industries. [0003] The synthetic method of the N-substituted phthalimide compound of prior art mainly is: react phthalimide and potassium hydroxide to generate potassium salt, take dimethylformamide as reaction solvent, Formed with the corresponding halide. And the preparation method for the phthalimide that is used as raw material mainly comprises carbon amine method, liquid ammonia method and urea method. Wherein, the carbon amin...

Claims

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Application Information

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IPC IPC(8): C07D209/48B01J31/02
CPCB01J31/0235B01J31/0279C07D209/48
Inventor 王兵波张森王伟张晓弟宋立雪
Owner 内蒙古源宏精细化工有限公司
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