Hydrochloric Acid → HCID 86671863, compound

Participants

Reaction Steps

A mixture of 10.5 g (0.02 mol) of 4-(N-methylperfluorobutanesulfonamidomethyl)-4′-chloromethylbiphenyl, and 1.90 g (0.024 mol) thiourea in 100 mL methyl ethyl ketone was stirred and heated at reflux. The initial solution became cloudy and by 1 hr a white precipitate formed. The mixture was heated for 17 hr, cooled, and filtered. The product (8.2 g) was heated in 150 mL boiling ethanol under N2 and treated with 8 g (0.1 mol) 50% NaOH and heated for 20 hr. The resulting hazy solution was cooled, treated with 20 mL 10% HCl, and poured into 200 mL water to give a white solid. This was taken up in methylene chloride, dried over MgSO4, and stripped to 7.0 g of the desired product.

Provenance & Evidence