Tetrafluoroboric acid → HCID 15869798, compound

Participants

Reaction Conditions

Reaction Steps

1.12 g (5.0 mmol) of 6-amino-1-(3-chloropropionyl)indoline (prepared as described in Preparation 6) were suspended in 20 ml of 6N aqueous hydrochloric acid, and a solution of 380 mg (5.5 mmol) of sodium nitrite in 5 ml of water was added to the suspension while ice-cooling so that the internal temperature was maintained at 10° C. or lower. The mixture was then stirred while ice-cooling for 30 minutes. At the end of this time, 2.0 mg (8.4 mmol) of fluoboric acid (as a 42% w/v aqueous solution) were added to the mixture, and the resulting mixture was stirred at 0° C. for 1 hour. The precipitated salt was collected by filtration. This salt was dried over phosphorous pentoxide in a desiccator under reduced pressure by means of a vacuum pump overnight to obtain 1.23 g (3.8 mmol) of the title compound as a solid (yield: 76%).

Provenance & Evidence