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Production method of m-aminoacetanilide

A technology of aminoacetanilide and m-aminoacetanilide hydrochloride, which is applied in the field of preparation of m-aminoacetanilide, and achieves the effects of simple process flow, high total yield, and shortened dehydration and drying time

Active Publication Date: 2020-05-12
YANTAI ANOKY FINE CHEM CO LTD +6
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] In view of the deficiencies in the existing production process, the object of the present invention is to provide a production method of m-aminoacetanilide, which can easily solve the above two problems in the m-aminoacetanilide production process

Method used

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  • Production method of m-aminoacetanilide
  • Production method of m-aminoacetanilide

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Embodiment 1～12

[0024] 1. Neutralization - 500mL beaker + 100g hydrochloride + 90mL water (all or part of the neutralization mother liquor from the previous batch was applied from the second batch), the temperature was raised to 50°C, and 32% liquid caustic soda was added dropwise , to pH=8~9, continue to stir at 60~65°C for 10 minutes, retest and adjust pH=8~9 with liquid caustic soda.

[0025] 2. Layering——The neutralized material is transferred into the separatory funnel, and settles for 10-15 minutes. The oil phase of the first batch is in the lower layer, and the oil phase is in the upper layer from the second batch. The oil phase is separated, and finally centralized distillation Dehydration treatment. The first batch of mother liquor is all applied mechanically as the second batch of neutralization bottom water, the second batch of mother liquor is all applied mechanically as the third batch of neutralization bottom water (a small amount of salt has been precipitated), the third batch ...

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Abstract

The invention discloses a production method of m-aminoacetanilide, which comprises the following steps: 1, proportionally adding m-aminoacetanilide hydrochloride and mechanically applying a mother solution into a reaction kettle, heating the raw materials to 30-100 DEG C, and neutralizing the system with a sodium hydroxide solution until the reaction endpoint is 7-10; 2, performing liquid-liquid sedimentation layering within the temperature range of 40-100 DEG C, thereby preparing a lower-layer product and an upper-layer product; 3, separating salt from the mother liquor in the lower-layer product, filtering to remove salt while hot, and applying the mother liquor in the next batch; and 4, transferring the oil phase in the upper-layer product into a distillation kettle, and carrying out vacuum distillation dehydration to obtain a finished product with qualified water content, wherein the finished product can be directly used for synthesizing m-acetamido-N,N-dimethoxycarbonyl methylaniline. The method is simple in technological process, simple to operate and control, low in wastewater yield and high in total yield, and particularly, the dehydration and drying time of the product isgreatly shortened.

Description

technical field [0001] The invention belongs to the field of preparation of organic chemical dye intermediate products, and in particular relates to a preparation method of m-aminoacetanilide. Background technique [0002] Aminoacetanilide is a very important coupling component intermediate in disperse dyes. Mainly used in the synthesis of m-acetamido-N,N-dimethoxycarbonylmethylaniline (referred to as A017), m-acetamido-N,N-diethylaniline and m-acetamido-N,N-diacetoxyethyl Aniline, etc. Traditional m-aminoacetanilide production method: use m-aminoacetanilide hydrochloride as raw material, neutralize with sodium hydroxide solution, then cool, crystallize, filter, wash, and dry to obtain the finished product. [0003] Specific as figure 1 As shown, there are following deficiencies in the existing preparation scheme: [0004] 1. The mother liquor can only be used for about 2 to 3 times, and must be discarded when the solubility of sodium chloride and sodium acetate is close...

Claims

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Application Information

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IPC IPC(8): C07C233/43C07C231/12C07C231/22
CPCC07C231/12C07C231/22C07C233/43
Inventor 曲美君戴杰李连伟渠晗张永明刘祥庆辛森森赵德禄潘伟林乐杭
Owner YANTAI ANOKY FINE CHEM CO LTD
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