Methanol → Acrylate

HRID 1886766

Reaktionsgleichung

Reaktionsgleichung von HRID 1886766
[OH2:1].CO.[OH:4][CH2:5][C:6]([CH2:19][OH:20])([CH2:9][O:10][CH2:11][C:12]([CH2:17][OH:18])([CH2:15][OH:16])[CH2:13][OH:14])[CH2:7][OH:8]>C(OC)(=O)C=C.OC1C=C(S(O)(=O)=O)C=CC=1C.C1(C)C=CC(S(O)(=O)=O)=CC=1.S([O-])([O-])(=O)=O.[Cu+2].C1(C)C=CC=CC=1>[C:17]([O-:18])(=[O:1])[CH:12]=[CH2:15].[OH:14][CH2:13][C:12]([CH2:17][OH:18])([CH2:11][O:10][CH2:9][C:6]([CH2:19][OH:20])([CH2:7][OH:8])[CH2:5][OH:4])[CH2:15][OH:16]

Komponenten

10

Edukt 3

HCID 887MethanolHCID 962WaterHCID 31352Dipentaerythritol

Produkt 2

HCID 25188AcrylateHCID 31352Dipentaerythritol

Reagenzien, Katalysatoren, Lösungsmittel 5

HCID 1140TolueneLösungsmittel2×HCID 6101p-Toluenesulfonic acidLösungsmittelHCID 7294Methyl AcrylateLösungsmittelHCID 24462Copper SulfateLösungsmittelHCID 124969923-Hydroxy-4-methylbenzenesulfonic acidLösungsmittel

Reaktionsbedingungen

Temperatur
100 °C

Versuchsvorschrift

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.

Aufarbeitung

  1. distillationwere distilled out
  2. customAfter the finish of the reaction

Quellen und Nachweise

ORD-Eintrag
ord-47b40a78ad204313bb5b7af03e03fabb
Quelldatensatz
uspto-grants-2013_08
Patentnummer
US08501391B2

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