Methylparaben → HCID 20571321, compound

Participants

Reaction Steps

In a six-liter flask equipped with stirrer, reflux condenser and thermometer, 608.6 g (4 moles) of 4-hydroxybenzoic acid methyl ester was suspended in 3.5 liters of methyl glycol, and by the addition of 160 g (4 moles) of sodium hydroxide in 160 ml of water was transformed to a solution of the phenolate. Then, at about 35°-40° C., with stirring, 981.3 g (2 moles) of 1,4-bis-(chloromethyl)-2,3,5,6-tetrabromobenzene was put in, and the reaction mixture was raised steadily to the boiling temperature, with stirring. After an internal temperature of about 90° C. was reached, reaction started, with the formation of a colorless, voluminous precipitate. The reaction mixture, after becoming increasingly thick, became thinner again at the boiling temperature. It was refluxed for 1.5 hours, then cooled down to room temperature; the precipitate was suction filtered and washed free of sodium chloride with water, and dried.

Provenance & Evidence