Ethyl Acetate → HCID 68693305, compound

Participants

Reaction Conditions

Reaction Steps

A mixture of (2S,5R)-methyl 2,4-dibenzyl-5-methylpiperazine-1-carboxylate (0.28 g, 0.83 mmol), phosphorous oxychloride (5.0 ml) and phosphorous pentoxide (0.48 g, 1.6 mmol) was stirred at 100° C. under nitrogen overnight. The reaction was removed from the heat, quenched with ice, and brought to pH 7 to 8 with 1 N NaOH. Extraction with EtOAc (3×) and washing the combined organic layers with brine and drying over MgSO4 afforded 0.11 g of crude product after evaporation of the solvent. Flash chromatography (SiO2, CH2Cl2 to 60% EtOAc in CH2Cl2) afforded pure product (47 mg, 19% yield). MS (ESI) 307 (M+H).

Provenance & Evidence