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A kind of synthetic method of β-iodoformic acid ester compound

A technology of ester compounds and synthesis methods, which is applied in the field of synthesis of organic compounds, can solve the problems of high toxicity, environmental pollution costs, etc., and achieve the effects of simple operation, environmental friendliness, and mild reaction conditions

Active Publication Date: 2020-06-23
ZHEJIANG UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] In order to solve the problems of high toxicity, environmental pollution and high cost in the current method for synthesizing β-iodate compounds, the present invention proposes a method for preparing β-iodoformate compounds. The synthetic method of the present invention overcomes the Disadvantages of existing technology

Method used

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  • A kind of synthetic method of β-iodoformic acid ester compound
  • A kind of synthetic method of β-iodoformic acid ester compound
  • A kind of synthetic method of β-iodoformic acid ester compound

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030]

[0031] Add 2mmol (0.208g) styrene and 2.2mmol (0.3652g) potassium iodide into a 50mL three-necked flask, then add 10mL formic acid as a solvent, and then add 0.8g bromate intercalated zinc aluminum hydrotalcite ZnAl-BrO 3 - -LDHs, magnetically stirred at 25°C for 3 hours, followed by TLC to complete the reaction. After the reaction, the obtained reaction liquid was centrifuged at 6500r / min to remove the zinc-aluminum hydrotalcite solid, and the obtained liquid was placed in a separatory funnel. Dichloromethane and deionized water were added, and the organic matter obtained from the reaction was extracted into the dichloromethane phase. Column chromatography silica gel is added to the resulting solution, the solvent is distilled off under reduced pressure, and the remaining mixture is separated by column chromatography. A mixed solvent of petroleum ether and ethyl acetate with a volume ratio of 10:1 is used as the eluent to collect the products containing The eluent is e...

Embodiment 2

[0034]

[0035] Add 2mmol (0.366g) 4-bromostyrene and 2.2mmol (0.3652g) potassium iodide into a 50mL three-necked flask, then add 10mL formic acid as a solvent, and then add 0.8g bromate intercalated zinc aluminum hydrotalcite ZnAl-BrO 3 - -LDHs, magnetically stirred at 50°C for 3 hours, followed by TLC to track the reaction to completion. After the reaction, the obtained reaction liquid was centrifuged at 6500r / min to remove the zinc-aluminum hydrotalcite solid, and the obtained liquid was placed in a separatory funnel. Dichloromethane and deionized water were added, and the organic matter obtained from the reaction was extracted into the dichloromethane phase. Column chromatography silica gel is added to the resulting solution, the solvent is distilled off under reduced pressure, and the remaining mixture is separated by column chromatography. A mixed solvent of petroleum ether and ethyl acetate with a volume ratio of 10:1 is used as the eluent to collect the products containin...

Embodiment 3

[0038]

[0039] Add 2mmol (0.277g) 4-chlorostyrene and 2.2mmol (0.3652g) potassium iodide into a 50mL three-necked flask, add 10mL formic acid as solvent, and then add 0.8g bromate intercalated zinc aluminum hydrotalcite ZnAl-BrO 3 - -LDHs, magnetically stirred at 50°C for 3 hours, followed by TLC to track the reaction to completion. After the reaction, the obtained reaction liquid was centrifuged at 6500r / min to remove the zinc-aluminum hydrotalcite solid, and the obtained liquid was placed in a separatory funnel. Dichloromethane and deionized water were added, and the organic matter obtained from the reaction was extracted into the dichloromethane phase. Column chromatography silica gel is added to the resulting solution, the solvent is distilled off under reduced pressure, and the remaining mixture is separated by column chromatography. A mixed solvent of petroleum ether and ethyl acetate with a volume ratio of 10:1 is used as the eluent to collect the products containing The...

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Abstract

The invention discloses a synthetic method of beta-iodine formate compounds shown as formula II in the description. Styrene compounds shown as formula I in the description and taken as raw materials, zinc-aluminium hydrotalcite ZnAlBrO3<->-LDHs intercalated with bromate taken as an oxidizing agent and an iodide taken as a reducing agent are subjected to a reaction in formic acid for 1-6 h, an obtained reaction liquid is subjected to aftertreatment, and the beta-iodine formate compounds shown as the formula II are obtained. Formic acid not only provides an acid chemical reaction environment, but also participates in addition and esterification directly as a nucleophilic reagent, and addition and esterification belong to atom-economic reactions; the iodine source used in the method is simple and available, reaction conditions are mild and environmentally friendly, and operation is simple.

Description

[0001] (1) Technical field [0002] The invention relates to a method for synthesizing organic compounds, in particular to a method for synthesizing β-iodoformate compounds. [0003] (2) Background technology [0004] The ortho-difunctionalization reaction of carbon-carbon double bonds is an important type of reaction in the field of organic chemistry, especially β-iodoformate compounds are an important reaction intermediate in organic synthesis, which can be obtained by various transformations. Drug molecules and active natural products. For example: due to the low bond energy of the carbon-iodine bond, the structure can undergo cross-coupling reaction under palladium catalysis to increase the carbon chain; the formate structure can undergo aminolysis, converted to amide, and further converted to other Of a variety of organic matter. [0005] At present, there are very few methods for the synthesis of β-bromoformate reported at home and abroad, and there are mainly the following met...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C67/05C07C69/63
CPCC07C67/05C07C69/63
Inventor 王力耕章华隆余琴
Owner ZHEJIANG UNIV OF TECH
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