Reaktion #5146

Reaktionsgleichung

methacryloyl chloride

2-bromo-4-2-hydroxyethoxymethylthiophene

pyridine

acetonitrile

water

→

2-bromo-4-thienyl-methoxyethyl methacrylate

Lösungsmittel

ethyl acetate

Reaktionsbedingungen

Aufarbeitung

1. 1
   workup.STIRRINGAfter stirring the mixture for one hour
2. 2
   ExtraktionThe ethyl acetate layer was extracted
3. 3
   Einengenconcentrated
4. 4
   Sonstigepurified by column chromatography

Vorschrift

While stirring a mixture of 0.1 mol of 2-bromo-4-2-hydroxyethoxymethylthiophene, 0.1 mol of pyridine, and 100 ml of acetonitrile at a temperature of lower than 10° C., 0.1 mol of methacryloyl chloride was added dropwise to the mixture over a period of 30 minutes. After stirring the mixture for one hour, 200 ml of ethyl acetate and 200 ml of water were added to the mixture. The ethyl acetate layer was extracted, concentrated, and purified by column chromatography to provide 22.1 g of 2-bromo-4-thienyl-methoxyethyl methacrylate (5-A).

Quelle