Hydrochloric Acid → HCID 12524399, compound

Participants

Reaction Conditions

Reaction Steps

9.5 mL of concentrated hydrochloric acid, 65 mL of pure water, and 6.0 g (35 mmol) of 2-bromoaniline were added to a 200-mL four-necked flask, and they were then dissolved by heating. The obtained solution was cooled to 0° C. Thereafter, an aqueous solution of 2.46 g (35.1 mmol) of sodium nitrite that had previously been dissolved in 7.5 mL of pure water was added dropwise thereto over approximately 10 minutes. The reaction solution that was first in a gruel-like state was converted to a light yellow transparent liquid by stirring it for 30 minutes. Subsequently, 12.5 g (59.8 mmol) of a 42-mass-% HBF4 aqueous solution was added dropwise thereto over approximately 5 minutes. As a result, light yellow crystals were immediately precipitated. The reaction solution was stirred for 30 minutes, and the crystals were then filtrated with a glass filter. The resultant was washed with 30 mL of pure water, and was then washed with a mixed solution of 8 mL of methanol and 32 mL of ether. Thereafter, the resultant was dried under a reduced pressure, so as to obtain 4.5 g of 2-bromobenzenediazonium tetrafluoroborate in the form of white crystals (yield: 48%).

Provenance & Evidence