Sulfuric Acid → HCID 13651711, compound

Participants

Reaction Steps

320 parts of methacrylic acid, 4 parts of p-toluene-sulfonic acid, 1 parts of copper-II chloride and 1.6 parts of hydroquinone monomethyl ether are dissolved in 1,200 parts of chloroform in a reaction vessel equipped with a reflux condenser and stirrer, and the solution is heated to the boil. A solution of 344 parts of hydroxypivalaldehyde in 1,200 parts of chloroform is run into the boiling solution over 4 hours. After this addition, 4 parts of 96% strength sulfuric acid are added and the water formed during the reaction is distilled off azeotropically. After completion of the reaction, and after cooling, the reaction mixture is washed with dilute aqueous sodium bicarbonate solution. After distilling off the chloroform under reduced pressure until the boiling point reaches 45° C., the residue is distilled in a thin film evaporator at 95° C./0.4 mm Hg. 274 parts of methacryloxypivalaldehyde (48% of theory, based on hydroxyaldehyde) of boiling point 51°-56° C./0.3 mm Hg are obtained. Analyses:

Provenance & Evidence