Sulfuric Acid → HCID 86739519, compound

Participants

Reaction Conditions

Reaction Steps

25.6 kg of 4-chloro-3-nitrophenylmethylsulfone are stirred slowly into 4 kg of 30% aqueous sodium hydroxide and the mixture is diluted continuously with water to a volume of about 50 liters. The reaction mixture is heated to 90° C. and then a further 29 kg of 30% aqueous sodium hydroxide are added, with stirring, over 3 to 4 hours. The mixture is then heated for 90 minutes to 103° C. After it has cooled to about 60° C., the solution is adjusted with 16% sulfuric acid to a pH value of about 1.5, whereupon the product precipitates. The precipitate is isolated by filtration, washed and recrystallised from ethanol. Yield: 24 kg of colourless crystals with a melting point of 166°-168° C.

Provenance & Evidence