Reaction #1973948

ord-47b40a78ad204313bb5b7af03e03fabb

Reaction equation

OCC(CO)(CO)COCC(CO)(CO)CO
dipentaerythritol
O
water
CO
methanol
OCC(CO)(CO)COCC(CO)(CO)CO
dipentaerythritol
C=CC(=O)[O-]
acrylate

Reagents

None

Conditions

Temperature
100°CELSIUS
Detailed conditions
See reaction.notes.procedure_details.

Workup

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

Procedure

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.

Source

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08501391B2uspto-grants-2013_08