Potassium Carbonate → HCID 76818454, compound

N-Methylpiperazine (104.16 g, 1041.6 mmol, 1.0 eq.) was added dropwise to a solution of 2-cyclohexen-1-one (100.0 g, 1041.6 mmol, 1.0 eq.) in ethanol (300 ml), and the resulting mixture was stirred for 5 hours at RT. The reaction solution was diluted with ethanol (600 ml) and cooled to 0° C.; K2CO3 (172.48 g, 1249.9 mmol, 1.2 eq.) and NH2OH.HCl (86.7 g, 1249.9 mmol, 1.2 eq.) were added, and the mixture was stirred for 30 minutes at 0° C. and then heated to RT and stirred for a further 16 hours. The reaction mixture was filtered off over Celite and washed with ethanol (500 ml). The filtrate was concentrated under reduced pressure and the residue was taken up in THF (100 ml) and n-hexane (500 ml) and stirred for 3 hours. The resulting solid was filtered off and used in the next stage without being purified further. Yield: 54% (120.0 g, 568.7 mmol)

1. temperaturecooled to 0° C.
2. stirringthe mixture was stirred for 30 minutes at 0° C.
3. temperatureheated to RT
4. stirringstirred for a further 16 hours
5. filtrationThe reaction mixture was filtered off over Celite
6. washwashed with ethanol (500 ml)
7. concentrationThe filtrate was concentrated under reduced pressure
8. stirringn-hexane (500 ml) and stirred for 3 hours
9. filtrationThe resulting solid was filtered off
10. customwithout being purified further

ORD record

ord-23a6ce8037be4123b6eae0bf12138452

Source dataset

uspto-grants-2014_03

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US08680159B2