Sulfuric Acid → 3-(5,5-Dimethyl-1,3-dioxan-2-yl)-1-(4-ethoxyphenyl)butan-1-one

Participants

Reaction Conditions

Reaction Steps

2-Bromo-1-(4-ethoxyphenyl)ethan-2-one (5.0 kg) and N,N-bis(2-methylpropyl)-1-propenylamine (5.1 kg) were added to 20 liters of acetonitrile under an atmosphere of nitrogen and the mixture was stirred at around 50° C. for 1.5 hours. To the reaction mixture were added successively 20 liters of water, 5.0 kg of concentrated sulfuric acid, 3.2 kg of neopentyl glycol, and 0.5 kg of para-toluenesulfonic acid and the mixture was stirred at around 50° C. for 1.5 hours. After cooling the reaction mixture to the room temperature, crystals precipitated. These crystals were isolated by filtration to give 4.3 kg (yield 71%) of the title compound as white crystals.

Provenance & Evidence