Chloroform → HCID 19907295, compound

Participants

Reaction Conditions

Reaction Steps

A solution of sodium sulphite (78.6 g) in water (2000 cm3) was added dropwise to a cooled solution of propyl diethylphosphonodichloroacetate (95.7 g) in ethanol (408cm3) over a period of 70 minutes, the temperature of the mixture being maintained below 8° C. during the addition by external cooling. The mixture was stirred at 8° C. for 10 minutes, then without external cooling for a further 15 minutes. Chloroform (100cm3) was added and the mixture stirred vigourously for 3 minutes. The chloroform phase was separated and combined with further chloroform extracts of the aqueous phase, The combined organic layers were dried over anhydrous magnesium sulphate and the solvent evaporated under reduced pressure to give the crude product as a yellow oil from which volatile compounds were removed by storage under high vacuum. The crude product was purified by distillation under reduced pressure to give a colourless liquid (75.2 g)

Provenance & Evidence