Hydroxylamine → HCID 178482922, compound

Temperature

80 °C

A mixture of 3-(dimethylamino)pyrrolidine (1.1 g), p-fluorobenzonitrile (1.2 g), potassium carbonate (2.8 g) and acetonitrile (15 ml) was stirred at 80° C. for 12 h. The reaction solution was then filtered, and the precipitate was washed with acetonitrile, the solvent was removed in vacuo, and the residue was taken up again in ethyl acetate. The ethyl acetate phase was washed twice with water and then dried over sodium sulfate, and the solvent was removed in vacuo. The product obtained in this way was dissolved in abs. ethanol (48.7 ml), and hydroxylamine (1.4 ml) was added to the solution. The reaction mixture was heated under reflux for 12 h. The precipitate obtained after cooling the reaction solution was filtered off and washed with a little ethanol.

1. filtrationThe reaction solution was then filtered
2. washthe precipitate was washed with acetonitrile
3. customthe solvent was removed in vacuo
4. washThe ethyl acetate phase was washed twice with water
5. dry with materialdried over sodium sulfate
6. customthe solvent was removed in vacuo
7. customThe product obtained in this way
8. dissolutionwas dissolved in abs
9. temperatureThe reaction mixture was heated
10. temperatureunder reflux for 12 h
11. customThe precipitate obtained
12. temperatureafter cooling the reaction solution
13. filtrationwas filtered off
14. washwashed with a little ethanol

ORD record

ord-2ae9163e5308461eb077ca88e1b9ce5e

Source dataset

uspto-grants-2008_01

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US07319108B2