Sodium Cyanide → HCID 18768930, compound

Temperature

60 °C

To a dry 250 mL round bottom flask set with a condenser was added sodium cyanide (0.786 g, 16.03 mmol), ammonium chloride (0.904 g, 16.9 mmol) and NH3/MeOH (2.0 M, 15.36 mL, 30.7 mmol). To the mixture was added 1-(3,3-dimethyl-butyl)-pyrrolidin-3-one (2.60 g, 15.36 mmol) and MgSO4 (2.5 g). The mixture was heated at 60° C. in an oil bath and stirred for 4 h. The mixture was cooled to room temperature and filtered to remove the insolubles, the filtrate was concentrated to dryness and the residue was dissolved in EtOAc/Et2O and filtered through a pad of diatomaceous earth then concentrated to dryness to give the title compound in (1.5 g, 51% yield). The crude compound was used in the next step without further purification.

1. customTo a dry 250 mL round bottom flask set with a condenser
2. temperatureThe mixture was cooled to room temperature
3. filtrationfiltered
4. customto remove the insolubles
5. concentrationthe filtrate was concentrated to dryness
6. dissolutionthe residue was dissolved in EtOAc/Et2O
7. filtrationfiltered through a pad of diatomaceous earth
8. concentrationthen concentrated to dryness

ORD record

ord-62b50ad5f6c54bf3b2a3393f94a65127

Source dataset

uspto-grants-2001_11

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US06313117B1