Potassium Carbonate → 4-(4-(4-Chlorophenyl)piperazin-1-yl)butanenitrile

To a solution of 4-bromobutanenitrile (1.50 g, 10.17 mmol) in dimethyl formamide (20 ml) were added 1-(4-chlorophenyl)piperazine (2.0 g, 10.17 mmol) and potassium carbonate (2.81 g, 20.34 mmol) at room temperature and the reaction mixture was stirred for 3 h at same temperature. The progress of the reaction was monitored by TLC. The reaction mixture was diluted with water (50 ml) and the aqueous layer was extracted with ethyl acetate (3×50 ml). The combined organic layer was dried over anhydrous sodium sulphate. The solvent in the organic layer was removed under reduced pressure to obtain a crude product, which was purified by column chromatography over silica gel (100-200 mesh) using 10% ethyl acetate in hexane to yield the title compound (2.32 g, 86% yield).

1. extractionthe aqueous layer was extracted with ethyl acetate (3×50 ml)
2. dry with materialThe combined organic layer was dried over anhydrous sodium sulphate
3. customThe solvent in the organic layer was removed under reduced pressure
4. customto obtain a crude product, which
5. customwas purified by column chromatography over silica gel (100-200 mesh)

ORD-Eintrag

ord-cbd0d717a5f94c099fbf5a179549cccc

Quelldatensatz

uspto-grants-2016_06

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US09359367B2