Hydrochloric Acid → HCID 12524399, compound

Temperature

0 °C

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%).

1. dissolutionthey were then dissolved
2. temperatureby heating
3. additionwas added dropwise
4. waitover approximately 5 minutes
5. customAs a result, light yellow crystals were immediately precipitated
6. stirringThe reaction solution was stirred for 30 minutes
7. filtrationthe crystals were then filtrated with a glass
8. filtrationfilter
9. washThe resultant was washed with 30 mL of pure water
10. washwas then washed with a mixed solution of 8 mL of methanol and 32 mL of ether
11. customThereafter, the resultant was dried under a reduced pressure

ORD record

ord-19fd51b6912d425d8fe757fac8db37f0

Source dataset

uspto-grants-2012_06

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US08198471B2