Water → HCID 22449363, compound

Participants

Reaction Conditions

Reaction Steps

A suspension of sodium hydride (12.5 g) in tetrahydrofuran (188 mL) was cooled to 0° C. A solution of malononitrile (10.3 g) in tetrahydrofuran (65 mL) was added dropwise thereto over a period of 1 hour. After stirring the reaction mixture at room temperature for 1 hour, it was again cooled to 0° C., and then a solution of 2-phenylacetyl chloride (24.2 g) in tetrahydrofuran (52 mL) was added dropwise thereto over a period of 80 minutes. After stirring the reaction mixture at room temperature for 49 hours, water (26 mL) was added to the reaction solution. The solvent was distilled off under reduced pressure, diethyl ether (130 mL) and 1 mol/L hydrochloric acid (130 mL) were added to the residue and extraction was performed with diethyl ether. The organic layer was washed with saturated brine and dried over anhydrous sodium sulfate, and then the solvent was distilled off under reduced pressure to obtain the title compound as a crude product (31.2 g).

Provenance & Evidence