Method for synthesizing aryl oxide chloride by using phenol chloride and alkyl chloride
A technology for dichloro aryl ether and dichloro phenol, which is applied in the field of preparing dichloro aryl ether, can solve the problems of long reaction time, decreased yield and purity, and increased side reactions such as hydrolysis, and achieves high purity and accelerated speed. Speed, simple process effect
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Embodiment 1
[0022] Take 16.5g of 2,4-dichlorophenol, 7g of NaOH, 1.1g of potassium iodide, and 0.16g of cetyltrimethylammonium bromide into the reactor, and add 20ml of water. Install a reflux condenser, a stirring device, a dripping device and a thermometer on the reactor, heat and dissolve 2,4-dichlorophenol, the temperature rises to 75°C, and start to drop 11.8g of chloroisocyanate through the dropping funnel Propane, control the temperature at 75-85°C when dropping, and control the dropping speed within 2 hours. After the dropping, reflux for 5 hours, then add 1g NaOH, and then reflux for 2 hours. After cooling, discharge the material and pass through 2% NaOH After the aqueous solution was washed, the liquids were separated, and the organic layer was distilled to remove chloroalkane, and then 17.6 g of the product 2,4-dichlorophenylisopropyl ether was obtained by distillation under reduced pressure, with a yield of 82%. The product was analyzed by gas chromatography and had a purity of...
Embodiment 2
[0024] Take 16.5g of 2,4-dichlorophenol, 6g of NaOH, 1.1g of potassium iodide, and 0.16g of cetyltrimethylammonium bromide into the reactor, and add 20ml of water. Install a reflux condenser, a stirring device, a dripping device and a thermometer on the reactor, heat and dissolve 2,4-dichlorophenol, the temperature rises to 90°C, and start to add 15.7g of chloroisocyanate dropwise through the dropping funnel. When adding propane, control the temperature at 78-90°C, and control the dropping speed within 2 hours. After the dropping, reflux for 6 hours, then add 2g NaOH, and then reflux for 2 hours. After cooling, discharge the material and pass through 2% NaOH After the aqueous solution was washed, the liquids were separated, and the organic layer was distilled to remove chloroisopropane, and then the product 2,4-dichlorophenylisopropyl ether was obtained by distillation under reduced pressure, with a yield of 85%. The product was analyzed by gas chromatography for purity. 96%. ...
Embodiment 3
[0026] Take 16.5g of 2,4-dichlorophenol, 10g of NaOH, 1.4g of potassium iodide, and 0.09g of tetraethylammonium bromide, add them to the reactor, and add 30ml of water. Install a reflux condenser, a stirring device, a dripping device and a thermometer on the reactor, heat and dissolve 2,4-dichlorophenol, the temperature rises to 90°C, and start to drop 14.1g of chloroisocyanate through the dropping funnel Propane, when adding dropwise, control the temperature at 85-100°C, and control the dropping rate within 3 hours. After the dropwise addition, reflux reaction for 5 hours, then add 0.5g NaOH, and then reflux for 2 hours. After cooling, discharge the material and pass through 2% NaOH After the aqueous solution was washed and separated, the organic layer was distilled to remove the chloroalkane, and then distilled under reduced pressure to obtain 17.5 g of the product 2,4-dichlorophenylisopropyl ether, with a yield of 81.1%. The product was analyzed by gas chromatography and had...
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