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Method of preparing alpha-ketoamide with micro-reaction apparatus

A micro-reaction device and ketamide technology, which is applied in the preparation of carboxylic acid amides, chemical instruments and methods, and the preparation of organic compounds. It can solve the problems of low solubility and blocked reaction pipelines, and achieve strong mass transfer capacity and low side reactions. , The effect of product quality improvement

Active Publication Date: 2018-04-27
NANJING TECH UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Purpose of the invention: In order to solve the low solubility of metal catalysts in solvents in the prior art and cause blockage of reaction pipelines, the present invention provides a method for preparing α-ketoamides using a micro-reaction device

Method used

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  • Method of preparing alpha-ketoamide with micro-reaction apparatus
  • Method of preparing alpha-ketoamide with micro-reaction apparatus
  • Method of preparing alpha-ketoamide with micro-reaction apparatus

Examples

Experimental program
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Effect test

Embodiment 1

[0037] use figure 1Preparation of α-ketoamide with a micro-reaction device: Weigh 1 g (0.006 mol) of ferric chloride powder and 7.7 g (0.048 mol) of 2,2'-bipyridine in a tank reaction filled with 30 mL of dichloromethane In the container, it is the raw material A, the heating temperature is 30 ° C, and the reaction is carried out for 3 hours. After the reaction, the reaction liquid is filtered through a filter to obtain a clear liquid. Weigh 1.25g (0.008mol) of 2,2,6,6,-tetramethylpiperidine oxide, 12.31g (0.1mol) of α-methylbenzyl alcohol, 11.81g (0.1mol) of p-aminobenzene Nitrile and 15.82g (0.2mol) of pyridine were dissolved in 60mL of dichloromethane, which was raw material B. Stir and mix the clear liquid and raw material B in the liquid storage tank to obtain a mixed liquid, feed nitrogen back pressure to 10 bar into the Corning reactor, switch to oxygen, and pump the mixed liquid into the Corning reactor at the same time. Keep the reaction temperature at 40°C, the flo...

Embodiment 2

[0039] The preparation method is the same as in Example 1, except that the heating temperature of ferric chloride powder and 2,2'-bipyridine in the tank reactor is 45°C, and the reaction is carried out for 3 hours. Through high-performance liquid chromatography analysis, in this reaction, the conversion rate of the α-ketoamide products generated is 94%.

Embodiment 3

[0041] The preparation method is the same as in Example 1, except that the reaction temperature in the Corning reactor is 45°C. According to high-performance liquid chromatography analysis, in this reaction, the conversion rate of the α-ketoamide products generated is 92%.

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Abstract

The invention discloses a method of preparing alpha-ketoamide with a micro-reaction apparatus, which includes the following steps: 1) mixing an alpha-methyl benzyl alcohol compound, an amine compound,an acid binding agent, 2,2,6,6-tetramethyl piperidine oxide and dichloromethane to obtain a heterogeneous solution; 2) mixing the heterogeneous solution with an organic iron catalyst solution to forma mixture solution, and respectively meanwhile pumping the mixture solution and oxygen gas into a micro-reactor in the micro-reaction apparatus to form a gas-liquid-solid mixture, and performing a reaction, after the reaction is finished, collecting an effluent liquid to obtain the alpha-ketoamide (III). With the organic iron catalyst for catalytically synthesizing the alpha-ketoamide, mixing status of the reactants is improved; the organic iron catalyst is better than ferric trichloride in solubility in the solvent, so that a problem of pipe blocking due to aggregation of ferric trichlorideparticles, thus accelerating homogenization of the system. The organic iron catalyst enables reaction conditions to be more gentle, reaction temperature being only 25-45 DEG C.

Description

technical field [0001] The invention belongs to the technical field of chemical synthesis and relates to the preparation of α-ketoamides, in particular to a method for preparing α-ketoamides using a micro-reaction device. Background technique [0002] α-Ketoamide is the core skeleton structure of many drugs and natural products. It is a class of compounds with a bifunctional structure, containing a carbon-nitrogen bond and two carbon-oxygen double bonds, and has multiple reaction centers. It plays an important role in synthesis, biochemistry, polymer materials, natural products, etc. [0003] Metal catalysis is an important method in organic synthesis, and there are many reports on the metal catalyzed synthesis of α-ketoamides. In organometallic catalyzed synthesis methods, heavy metal catalysts such as palladium, copper, and gold are the most important. Metal catalysts have good reactivity and wide applicability in oxidation reactions. The use of iron salts to catalyze th...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C231/10C07C235/78B01J31/22
CPCC07C235/78B01J31/1815B01J2531/842
Inventor 郭凯曾雨方正刘成扣欧阳平凯
Owner NANJING TECH UNIV
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