Benzyl Chloride → HCID 178418301, compound

Participants

Reaction Conditions

Reaction Steps

A mixture of ammonium phosphinate (9.18 g) and hexamethyldisilazane (25 mL) was heated at 110° C. for 2 hours. The mixture was cooled in ice, dissolved in dry dichloromethane (120 mL), benzyl chloride (20 g; 14 mL) was added and the mixture allowed to warm to room temperature and stirred 18 hours. The solution was filtered, the solvent evaporated, the residue azeotroped with methanol (2×70 mL), dissolved in toluene (150 mL) containing n-butanol (30 mL) and the solution was boiled under reflux in a Dean and Stark water trap for 5 hours. The solvent was evaporated, the residue slurried with dichloromethane (120 mL), filtered and evaporated and the residue chromatographed on silica-gel in 1-2% methanol in dichloromethane to give the title compound as an oil.

Provenance & Evidence