Hydrochloric Acid → HCID 19385224, compound

Temperature

80 °C

A concentrated hydrochloric acid solution (120 mL) was added to a suspension of 4-amino-3-nitrobenzene trifluoride (20.06 g) and ethanol (400 mL) in air. The mixture was heated to 80° C. with stirring. After reduced iron (27.09 g) was gradually added thereto over a period of 15 minutes, the mixture was heated to reflux for 1 hour with stirring. After the mixture was cooled on ice, the resulting solution was neutralized with aqueous ammonium hydroxide and then extracted with dichloromethane. The extract was washed with water, concentrated, and purified by silica-gel column chromatography to yield 3,4-diaminobenzene trifluoride (12.495 g).

1. temperaturethe mixture was heated
2. temperatureto reflux for 1 hour
3. stirringwith stirring
4. temperatureAfter the mixture was cooled on ice
5. extractionextracted with dichloromethane
6. washThe extract was washed with water
7. concentrationconcentrated
8. custompurified by silica-gel column chromatography

ORD record

ord-a96406481a224ce591404bd0c86d8a4f

Source dataset

uspto-grants-2011_09

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US08022617B2