반응 #1973948

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dipentaerythritol

water

methanol

→

dipentaerythritol

acrylate

용매

methyl acrylate

3-hydroxy-4-methyl-benzenesulfonic acid

p-toluenesulfonic acid

copper sulfate

toluene

toluene

반응 조건

후처리

1. 1
   workup.DISTILLATIONwere distilled out
2. 2
   기타After the finish of the reaction

실험 절차

In a four-neck glass flask of 3 L in volume to which a reflux cooler, a water separator, an air introducing tube, a thermometer and a stirrer were attached, 203 g of methyl acrylate, 100 g of dipentaerythritol (purity: 95% or higher, made by Tokyo Chemical Industry Co., Ltd.), 6.3 g of 3-hydroxy-4-methyl-benzenesulfonic acid, 12.6 g of p-toluenesulfonic acid, 0.16 g of copper sulfate, and further 140 g of toluene as a solvent were charged. The mixture was stirred while nitrogen gas was blown in the flask, and heated at 100° C. for 2 hours. Thereafter, while the system interior was gradually depressurized and methanol produced by the transesterification and toluene as a solvent were distilled out, the reaction was performed finally at 200 mmHg for 6 hours. After the finish of the reaction, cleaning with an alkali aqueous solution and a neutralization operation were repeated to obtain an acrylate of dipentaerythritol as a reaction product.

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