Sodium Cyanide → HCID 45087748, Verbindung

KCN (1.26 g, 25.7 mmols), NaCN (2.78 mg, 42.7 mmols) and 18-crown-6 (793 mg, 3 mmols) were added to a CH3CN (60 ml) solution of the (5R)-5-(bromomethyl)-1-methylpyrrolidin-2-one (2.67 g, 13.9 mmols), and the mixture was heated for 44 hours under reflux. The inorganic matter was filtered off, and the filtrate was diluted with AcOEt (50 ml). The dilution was washed with a saturated aqueous solution (30 ml) of NaCl, and dried over MgSO4. The solvent was distilled off under reduced pressure, and then the residue was subjected to silica gel column chromatography (SiO2 100 g, MeOH—CHCl3 1:9 v/v) to obtain 2-((2R)-1-methyl-5-oxopyrrolidin-2-yl)ethanenitrile as a mixture (1.49 g) with impurities difficult to separate.

1. temperaturethe mixture was heated for 44 hours
2. temperatureunder reflux
3. filtrationThe inorganic matter was filtered off
4. additionthe filtrate was diluted with AcOEt (50 ml)
5. washThe dilution was washed with a saturated aqueous solution (30 ml) of NaCl
6. dry with materialdried over MgSO4
7. distillationThe solvent was distilled off under reduced pressure

ORD-Eintrag

ord-62925c6323f64817a9b385d6ad2d5f10

Quelldatensatz

uspto-grants-2005_09

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US06949553B2