Phosphorus oxychloride → HCID 18172454, compound

Participants

Reaction Steps

A solution of cyclohexanecarboxylic acid [2-(3-methoxyphenyl)ethyl]amide (1.000 g, 3.8 mmol) in POCl3 (7.0 ml, 75.1 mmol) was refluxed under N2 for 24 hr, then the cooled reaction mixture was slowly added to ice-water (30 ml) with stirring. The resulting mixture was extracted with EtOAc (3×20 ml), then the remaining aqueous layer was basified to pH 10 with concentrated ammonia (40 ml). This was extracted with CHCl3 (4×20 ml), then the combined extracts were dried over MgSO4 and concentrated in vacuo to give 0.270 g (93% yield) of yellow oil.

Provenance & Evidence