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PENTAERYTHRITOLDIALLYLETHER synthesis

7synthesis methods
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Yield:1471-17-6 87.6% ,1471-18-7 6.1% ,2590-16-1 5.3%

Reaction Conditions:

Stage #1: Pentaerythritolwith tetrabutylammomium bromide;sodium hydroxide in water at 90;Industrial scale;
Stage #2: 3-chloroprop-1-ene in water at 110;Industrial scale;

Steps:

3 Example 3

Put pentaerythritol, sodium hydroxide aqueous solution (50%), pentaerythritol triallyl ether, and tetrabutylammonium bromide into the reactor equipped with stirring, heating coil, condenser, and water separation tank. The feeding valve is heated to 90°C until the pentaerythritol is completely melted, and the stirring is turned on, and the stirring is uniform, and the propylene chloride is slowly added dropwise. Depending on the temperature of the kettle, gradually increase the rate of dripping. During the dripping process, the water must be continuously divided. The temperature of the kettle is kept rising throughout the dripping process. When the temperature rises to 110, the chloropropene is dripped to 80% for sampling and analysis. According to the analysis results Continue to add chloropropene dropwise and control the dropping time within 10-16 hours. After the addition, the reflux was maintained for two hours and the reaction was stopped. After keeping the temperature for half an hour, add 1250kg of water in the water separation tank to cool down and wash with stirring. When the temperature drops to 50°C, after stirring and washing for 30 minutes, separate the lower layer of water. The upper organic phase was distilled to remove light components, and then reduced to -0.095MPa to collect the 150-180°C fraction to obtain 4030kg of product, in which the content of pentaerythritol diallyl ether was 5.28%, the content of pentaerythritol triallyl ether was 87.64%, and the pentaerythritol tetraene The propyl ether content is 6.14%, and the total ether content is 99.06%; the molar yield based on pentaerythritol is 85.63%.

References:

CN111170836,2020,A Location in patent:Paragraph 0053-0063