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Chlorinated alkane photo-carbonylation reaction method at cadmium compound catalysis

A technology of carbonylation reaction and chlorinated alkanes, which is applied in the direction of chemical instruments and methods, physical/chemical process catalysts, carbon monoxide or formate reaction preparation, etc., to achieve the effect of low input cost, mild reaction conditions and high added value

Inactive Publication Date: 2008-08-20
DALIAN UNIV
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Problems solved by technology

[0002] Conventional carbonylation reactions of halogenated alkanes often take iodoalkanes and brominated alkanes as substrates, and most of them need to be carried out under the conditions of high temperature and high pressure or the use of noble metal catalysts (such as platinum, rhodium, palladium, etc.) (TakeuchiR et al., J. Org.Chem., 1989, 54 (8): 1831-1836), and there are few reports on the carbonylation reaction of chlorinated alkanes

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  • Chlorinated alkane photo-carbonylation reaction method at cadmium compound catalysis

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Embodiment Construction

[0012] The specific operation steps of the method of the present invention are as follows: place a 400W high-pressure mercury lamp inside a hollow interlayer quartz photoreactor, pass circulating water into the interlayer, and simultaneously put the entire reactor into a water tank filled with water to cool the lamp Source; 5ml of methanol solution containing chlorinated alkanes substrate and catalyst is added in the quartz test tube, the quartz test tube is close to the outer wall of the photoreactor, carbon monoxide or carbon dioxide is introduced into the reaction solution, and the pressure is kept constant at room temperature after replacement and deoxygenation. 0.1MPa, start the light source to irradiate the reaction solution for 25h, the illumination of the light source is 2.6×10 -2 W / m 2 , the distance from the center of the light source to the center of the reaction solution is 3.3×10 -2 m. With n-decane as internal standard, the product was analyzed by GC and GC-MS ...

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Abstract

The invention relates to a method for preparing methyl-carboxylate by photo-promoted carbonylation reaction of chloro alkane on the moderate condition of non-noble metal catalysis, under the catalysis of non-noble metal catalyst cadmium, making chloro alkane and CO or CO2 perform photo- promoted carbonylation reaction in the methanol to produce the methyl-carboxylate which increases one C as compared with the chloro alkane, where the chloro alkane in the reaction is chloro cyclohexane and / or 1-chloro octane; the catalyst is selected from (a) 4-20mmol / L CdI2, (b) combination of 5-20mmol / L CdCl2 and 4-20mmol / L NaI, or (c) combination of 5-20mmol / L Cd(NO3)2 and 4-20mmol / L NaI. And it adopts non-noble metal compound as catalyst and uses chloro alkane as substrate; and the reacting condition is moderate, the cost is low, and it is suitable for small-scale and high-added value methyl-carboxylate synthesis.

Description

technical field [0001] The invention relates to the preparation of carboxylate, in particular to a method for preparing methyl carboxylate from chlorinated alkanes through light-promoted carbonylation reaction under non-noble metal catalyzed mild conditions. Background technique [0002] Conventional carbonylation reactions of halogenated alkanes often take iodoalkanes and brominated alkanes as substrates, and most of them need to be carried out under the conditions of high temperature and high pressure or the use of noble metal catalysts (such as platinum, rhodium, palladium, etc.) (TakeuchiR et al., J. Org.Chem., 1989, 54(8): 1831-1836), and there are few reports on the carbonylation reaction of chlorinated alkanes. [0003] In recent years, light-promoted carbonylation of haloalkanes has attracted extensive attention due to its low requirements on reaction conditions. Watanabe et al. used platinum complexes as catalysts to study the light-promoted carbonylation of iodoal...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C67/38C07C69/75C07C69/24B01J27/138B01J27/25
Inventor 贾颖萍高大彬尹静梅周广运王宏伟
Owner DALIAN UNIV
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