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Method for preparing difluoro alkyl ether benzene

A technology of difluorobenzene alkyl ether and alkyl group is applied in the field of preparation of difluorobenzene alkyl ether to achieve the effects of low energy consumption, convenient post-processing and easy industrial production

Active Publication Date: 2007-07-25
SHANGHAI CHEMSPEC CORP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

There is no report on the method of preparing 2,3-difluorophenyl alkyl ether and 2,6-difluorophenyl alkyl ether respectively by using the same reaction route

Method used

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  • Method for preparing difluoro alkyl ether benzene
  • Method for preparing difluoro alkyl ether benzene
  • Method for preparing difluoro alkyl ether benzene

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] The preparation of embodiment 1 difluoroanisole

[0034] Add 67.3g (1.2mol) of potassium hydroxide, 240ml of toluene, 40.4g (1.26mol) of methanol into a 1000ml reaction flask, stir and mix and add 79.3g (0.6mol) of 1,2,3-trifluoro Benzene, keep warm for 4 to 5 hours after the dropwise addition; add 100ml of water to the reaction solution, stir for 15 minutes, and filter with suction. Dry over anhydrous magnesium sulfate, evaporate the solvent with a rotary evaporator, add the residue to the still, adjust the vacuum to 30mmHg, start heating to reflux, and wait for the reflux to stabilize at 85°C, start to extract fractions, and the reflux ratio is 1:2 , when the distillation temperature reached 90°C, began to collect 2,6-difluoroanisole fractions, and when the temperature reached 91°C, stopped the extraction to obtain 27g of colorless transparent liquid 2,6-difluoroanisole. GC analysis purity is 99.8%,

[0035] 1 H-NMR (CDCl 3 .500MHz) δppm: 6.80-6.95 (m, 3H), 3.84 (s,...

Embodiment 2

[0038] The preparation of embodiment 2 difluoroanisole

[0039] Add 84.2g (1.2mol) of potassium methylate and 240ml of toluene into a 1000ml reaction flask, stir and mix, then add 79.3g (0.6mol) of 1,2,3-trifluorobenzene dropwise at room temperature, and keep warm for reaction 4 ~5 hours; add 100ml of water to the reaction solution, stir for 15min, filter with suction, take the organic layer after the filtrate is allowed to stand and separate, wash with 5% sodium bicarbonate solution until neutral, dry over anhydrous magnesium sulfate, and use a rotary evaporator Evaporate the solvent, put the residue into the still, adjust the vacuum degree to 25mmHg, and start heating to reflux. After the reflux is stable at 80°C, start to extract the distillate. The reflux ratio is 1:2. When the distillation temperature reaches 90°C , began to collect 2,6-difluoroanisole fractions, and when the temperature reached 92°C, the extraction was stopped to obtain 31g of colorless transparent liqui...

Embodiment 3～7

[0040] The preparation of embodiment 3~7 difluoroanisole

[0041] Except for etherification reaction temperature and reaction time, other operating conditions are all the same as in Example 1, and the results are shown in Table 1.

[0042] Table 1

[0043]

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Abstract

This invention relates to a method for preparing difluorophenyl alkyl ether. The method comprises: adopting 1,2,3-trifluorobenzene as the raw material, etherifying with alkoxyl salt of alkali metal or alkaline earth metal, or etherifying with alkyl alcohol in the presence of alkali, and performing fractionation to obtain high-purity 2,3-difluorophenyl alkyl ether and 2,6-difluorophenyl alkyl ether. The method has such advantages as simple process, mild reaction conditions, low energy consumption, low equipment requirement, short reaction time, convenient post-treatment, and little environmental pollution. The target product has high purity and stable quality, and can be used as the intermediate of medicine.

Description

technical field [0001] The invention relates to a preparation method of difluorophenyl alkyl ether, in particular to a method for preparing 2,3-difluorophenyl alkyl ether and 2,6-difluorophenyl alkyl ether. Background technique [0002] 2,3-Difluorophenylalkyl ether and 2,6-difluorophenylalkyl ether are intermediates with increasingly wide uses, and are commonly used intermediates for the synthesis of liquid crystal compounds, pharmaceutical compounds and pesticide compounds. Disclosed in Chinese patent CN89101335 is the synthetic method of 2,3-difluorobenzene alkyl ether, and the feature of this method is to use organometallic reagent to make o-difluorobenzene deprotonate on 1-position, then react with electrophile or The 1-position is hydroxylated by the oxidation method and treated with an alkylating agent under basic conditions to obtain the corresponding 2,3-difluorophenyl alkyl ether. Most of the raw and auxiliary materials used in this method (especially organometall...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C41/01C07C43/225
Inventor 袁云龙金叠
Owner SHANGHAI CHEMSPEC CORP