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Oxime ether synthesis method

A technology for oxime ether and ketoxime, which is applied in the field of synthesizing oxime ether, can solve the problems of high production cost, high loss, high unit price, etc., and achieves the effects of avoiding corrosion, avoiding discharge, and improving yield

Inactive Publication Date: 2019-02-22
ZHEJIANG UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The unit price of the ionic liquid in this process is expensive, the loss is large, and the production cost is high

Method used

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  • Oxime ether synthesis method

Examples

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Embodiment 1

[0023] In a 1000ml autoclave, add 87g (1mol) methyl ethyl ketone oxime (purity: 98%), 54g (1mol) sodium methoxide, 300ml anhydrous DMF, pass into 60g (1.2mol) methylene chloride, Sealed reaction at 30°C for 6h. Cool to room temperature after the reaction, filter the reaction liquid, wash the filter residue with DMF, combine the filtrate and washing liquid, carry out precipitation and rectification, collect the fraction at 80-83°C, and obtain the pure product butanone-O-methyloxime Ether, the yield is 80%, and the purity is 99%.

Embodiment 2

[0025] Replace 87g (1mol) of methyl ethyl ketone oxime (99% in purity) with 73g (1mol) of acetone oxime (99% in purity), and collect fractions at 75-78°C during rectification. Other conditions and operating procedures are the same as in the examples 1. Obtain the pure product acetone-O-methyl oxime ether with a yield of 83% and a purity of 99%.

Embodiment 3

[0027] Replace 87g (1mol) methyl ethyl ketoxime (99% purity) with 101g (1mol) methyl propyl ketone oxime (purity 99%), collect fractions at 127~130°C during rectification, other conditions and operations The process was the same as in Example 1, and the pure product methyl propyl ketone-O-methyl oxime ether was obtained, with a yield of 75% and a purity of 99%.

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Abstract

The invention discloses an oxime ether synthesis method. The method comprises the steps as follows: putting ketoxime and organic base in the molar ratio being 1:(1-1.5) into a high-pressure reactor, adding an organic solvent, controlling the reaction temperature at 10-60 DEG C, introducing an alkylation reagent, conducting a reaction for 2-6 h, filtering a reaction solution after the reaction ends, after removing the solvent from filtrate, performing distillation or crystallization to obtain an oxime ether product; the chemical structural formula of oxime ether is shown in formula (I), whereinR1 and R2 independently represent C1-C3 alkyl; R is substituted benzyl or C1-C3 alkyl. An organic phase one-pot method process is adopted to replace a water phase stepped method process, oxime etherhydrolysis side reactions are avoided, the process operation is simplified, the reaction yield is increased, and discharge of wastewater is reduced.

Description

technical field [0001] The invention relates to a method for synthesizing oxime ethers. Background technique [0002] Oxime ethers and their derivatives are widely used in medicine and pesticides. For example, they are important intermediates for the preparation of alkoxyamines. At present, the methods for synthesizing oxime ethers mainly include the following three processes: [0003] The first one is Pan Zhongwen et al. (Fine Chemical Intermediates, 2007, 37(6), 17-21) introduced the acetone-O-ethyloxime ether aqueous phase one-pot process, that is, using water as solvent and sodium hydroxide As an acid-binding agent, acetone oxime reacts with diethyl sulfate, and the oxime ether product is obtained after liquid separation and rectification. This process is highly corrosive to equipment, produces more waste salt and waste water, and the raw material diethyl sulfate is more toxic. [0004] The second is the European patent (EPO158159) which introduces the water-phase step...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C249/12C07C251/38C07C251/52
CPCC07C249/12C07C251/38C07C251/52
Inventor 李小青张琛徐大旺许响生
Owner ZHEJIANG UNIV OF TECH
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