HCID 178418361, compound → 1-Aminoanthraquinone

Temperature

80 °C

To 100 parts of ethyleneglycol monomethyl ether (so called methyl-Cellosolve) there were added 5.0 parts of 1-hydroxylaminoanthraquinone and 0.25 part of Raney nickel. The reaction mixture was heated to 80°C over 30 minutes and maintained at 80°C for 4 hours, with stirring, while introducing thereinto 0.04 parts/hour of gaseous hydrogen. The reaction mixture was then purged of gaseous hydrogen with gaseous nitrogen, heated to 100°C and filtered while hot to separate the catalyst as residue. The filtrate was, while maintained at 80°C, added with 100 parts of water, with stirring, to precipitate crystals. The slurry thus formed was then cooled to room temperature and filtered. The residue was washed with 5 parts of methanol and dried to obtain 4.2 parts of 1-aminoanthraquinone of a purity of 97 %. In the filtrate there remained 0.1 part of 1-aminoanthraquinone dissolved.

1. temperaturemaintained at 80°C for 4 hours
2. additionwhile introducing
3. customThe reaction mixture was then purged of gaseous hydrogen with gaseous nitrogen
4. temperatureheated to 100°C
5. filtrationfiltered while hot
6. customto separate the catalyst as residue
7. temperaturewhile maintained at 80°C
8. additionadded with 100 parts of water
9. stirringwith stirring
10. customto precipitate crystals
11. customThe slurry thus formed
12. temperaturewas then cooled to room temperature
13. filtrationfiltered
14. washThe residue was washed with 5 parts of methanol
15. customdried

ORD record

ord-f42cafdf3ffe4cdc823468fe0469ad6a

Source dataset

uspto-grants-1976_06

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US03966775