Trifluoroacetic acid → HCID 86646942, compound

Participants

Reaction Steps

add 0.376 cm3 of trifluoroacetic acid to a solution of 0.250 g of 1,1-dimethylethyl 4-{2-[({6-[1-(2,6-dichloro-3-fluorophenyl)ethoxy]-1,3-benzothiazol-2-yl}carbamoyl)amino]ethyl}piperazine-1-carboxylate trifluoroacetate in 5 cm3 of dichloromethane. Continue stirring for 4 hours at a temperature close to 20° C. The reaction mixture is then evaporated to dryness under reduced pressure (2 kPa). The residue is taken up in 10 cm3 of water. The mixture obtained is adjusted to pH 9 with a 1N solution of sodium hydroxide and then extracted three times with 20 cm3 of ethyl acetate. The combined organic phases are dried over magnesium sulphate, then filtered and evaporated to dryness under reduced pressure (2 kPa). The white solid obtained is solidified in 5 cm3 of diisopropyl oxide, filtered and then dried under reduced pressure. We obtain 0.117 g of 1-{6-[1-(2,6-dichloro-3-fluorophenyl)ethoxy]-1,3-benzothiazol-2-yl}-3-(2-piperazin-1-ylethyl)urea trifluoroacetate in the form of a white powder, which has the following characteristics:

Provenance & Evidence