Ethanol → HCID 59304998, compound

Participants

Reaction Steps

2.60 g (7.36 mmol) of 4-(dibenzylamino)-2,6-difluorobenzoic acid are dissolved in 20 ml of dioxane. 2.42 g (8.83 mmol) of diphenylphosphyl azide and then 1.08 g (10.7 mmol) of triethylamine are added dropwise, and the mixture is stirred at RT for one hour. 6.0 ml of ethanol are then added, and the mixture is heated under reflux for 2 hours. The reaction solution is then concentrated and the residue is dissolved in dichloromethane. The solution is washed with semiconcentrated sodium bicarbonate solution and water and dried over sodium sulfate, and the solvent is removed under reduced pressure. The residue is purified by chromatography on silica gel (mobile phase: dichloromethane). The oil obtained is dissolved in a little dichloromethane. Addition of a little pentane and scratching yields crystals which are filtered off with suction.

Provenance & Evidence