A kind of production method of m-aminoacetanilide

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

Active Publication Date: 2022-04-15
YANTAI ANOKY FINE CHEM CO LTD +6
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  • 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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  • A kind of production method of m-aminoacetanilide
  • A kind of production method of m-aminoacetanilide
  • A kind of 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: step 1: put m-aminoacetanilide hydrochloride in a proportion into a reaction kettle, apply mother liquor mechanically, heat up to a temperature range of 30-100°C, Then use sodium hydroxide solution to neutralize to the end of the reaction, the end point of the reaction is in the pH range of 7 to 10; step 2: carry out liquid-liquid sedimentation and stratification in the temperature range of 40 to 100 ° C; obtain the lower layer product and the upper layer product; Step 3: Separate the salt in the lower product from the mother liquor, and filter while it is hot to remove the salt, and the mother liquor will be used in the next batch; Step 4: Move the oil phase in the upper product into a distillation kettle for vacuum distillation and dehydration to obtain a finished product with a qualified moisture content. It is directly used in the synthesis of m-acetamido-N,N-dimethoxycarbonylmethylaniline. This method has simple technological process, simple operation and control, low waste water generation and high total yield, especially the dehydration and drying time of the product is greatly 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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Patent Type & Authority Patents(China)
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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