Hydrofluoric Acid → HCID 13377161, compound

Participants

Reaction Conditions

Reaction Steps

0.5 mole of 1,1-dimethyl-3-(3-methyl-5-nitrobenzothiophen-7-yl)-triazene is introduced in portions into 10 moles of hydrofluoric acid. The apparatus is then closed, 5 bar of nitrogen are forced in and the mixture is warmed to 100° C. The nitrogen formed is let down continuously under 9 bar. When the reaction had ended (about 1 hour), the mixture is cooled to room temperature, the residual pressure is let down and excess HF is distilled off in vacuo. The residue is stirred in methylene chloride and the mixture is washed neutral with water and finally with NaHCO3 solution, dried and concentrated. The product is purified by recrystallisation from light petroleum.

Provenance & Evidence