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A method for melting and crystallizing separation and purification of o-iodoaniline

A technology of melting crystallization and o-iodoaniline, which is applied in the field of separation and purification of o-iodoaniline, can solve the problems of only 45% yield, easy deterioration, and low efficiency

Active Publication Date: 2020-10-23
GUIZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Direct substitution of o-iodoaniline is accompanied by the generation of isomer p-iodoaniline. In the preparation method of o-iodoaniline in patent 201610944091.3, it is mentioned that extraction crystallization, recrystallization and column chromatography separation are used for purification, but the efficiency Low, the yield is only 45%
However, o-iodoaniline is easy to deteriorate in a high-temperature environment, so it is not suitable for separation and purification by rectification.
At present, there are no relevant reports on the literature and invention patents of the use of melting crystallization technology to purify o-(p-) iodoaniline

Method used

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  • A method for melting and crystallizing separation and purification of o-iodoaniline
  • A method for melting and crystallizing separation and purification of o-iodoaniline

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] Embodiment 1: a kind of method that melt crystallization separates and purifies o-iodoaniline, comprises the following steps:

[0032] 1) Select a mixture of o-iodoaniline and p-iodoaniline, which accounts for 55% of the total mass fraction, as a raw material, and grind it into powder to obtain product A;

[0033] 2) Put product A into the crystallizer, then open the crystallizer, heat product A to 75°C to completely melt product A, and obtain product B;

[0034] 3) Cool product B at a rate of 5°C / h to make it crystallize, grow crystals for 0.5 hours after reaching the final crystallization temperature of 50°C, and then release the mother liquor to obtain product C;

[0035] 4) The product C is gradually heated up at a rate of 5°C / h to sweat until the final sweating temperature is 60°C, and sweat is released, and the remaining crystals are purified o-iodoaniline.

Embodiment 2

[0036] Embodiment 2: a kind of method that melt crystallization separates and purifies o-iodoaniline, comprises the following steps:

[0037] 1) Select a mixture of o-iodoaniline and p-iodoaniline, which accounts for 65% of the total mass fraction, as a raw material, and grind it into powder to obtain product A;

[0038] 2) Put product A into the crystallizer, then open the crystallizer, heat product A to 65°C to completely melt product A, and obtain product B;

[0039] 3) Cool product B at a rate of 4.1°C / h to crystallize it, grow crystals for 2 hours after reaching the final crystallization temperature of 42°C, and then release the mother liquor to obtain product C;

[0040] 4) The product C is gradually heated up at a rate of 4.1°C / h to sweat until the final sweating temperature is 50°C, and sweat is released, and the remaining crystals are purified o-iodoaniline.

Embodiment 3

[0041] Embodiment 3: a kind of method of melt crystallization separation and purification o-iodoaniline, comprises the following steps:

[0042] 1) Select a mixture of o-iodoaniline and p-iodoaniline, which accounts for 75% of the total mass fraction, as a raw material, and grind it into powder to obtain product A;

[0043] 2) Put product A into the crystallizer, then open the crystallizer, heat product A to 55°C to completely melt product A, and obtain product B;

[0044] 3) Cool product B at a rate of 3°C / h to crystallize it, grow crystals for 5 hours after reaching the final crystallization temperature of 33°C, and then release the mother liquor to obtain product C;

[0045] 4) The product C is gradually heated up at a rate of 3°C / h to sweat until the final sweating temperature is 40°C, and sweat is released, and the remaining crystals are purified o-iodoaniline.

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Abstract

The invention discloses a method for melting, crystallizing, separating and purifying iodoaniline. The method comprises the following steps: 1) grinding an iodoaniline and paraiodoaniline mixture rawmaterial into powder to obtain a product A; 2) putting the product A into a crystallizer, starting the crystallizer, heating the product A and completely melting the product A to obtain a product B; 3) cooling the product B to perform crystallization, growing the crystal after the crystallization final temperature is arrived, and discharging mother liquid to obtain a product C; and 4) heating andsweating the product C step by step until the sweating final temperature and discharging the sweat, wherein the residual crystal is the purified iodoaniline. The method provided by the invention has the characteristics of no need of organic solvent, environmental friendliness, high separation and purification efficiency, small loss amount of iodoaniline, low cost and high purity of the iodoaniline, and is suitable for industrialized popularization.

Description

technical field [0001] The invention relates to a method for separating and purifying o-iodoaniline, in particular to a method for separating and purifying o-iodoaniline by melt crystallization. Background technique [0002] O-iodoaniline and its derivatives can be used as raw materials for the preparation of indole anticancer drugs. With suitable catalysts, various indole drug intermediates can be efficiently synthesized. With its wide application in the fields of medicine, pesticides and materials, The demand for o-iodoaniline will continue to rise. Indole compounds are a class of heterocyclic derivative alkaloids with significant physiological activity. In the development of new drugs, indole structures are often given priority as lead compounds. O-iodoaniline can react with alkynes to prepare indole by Larock-Castro synthesis, or obtain indole derivatives by Heck method under palladium catalysis. O-iodoaniline and its derivatives are often used in the preparation of i...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C209/86C07C211/52
CPCC07C209/86C07C211/52
Inventor 李天祥朱静许奎
Owner GUIZHOU UNIV
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