Ethanol → HCID 13282598, compound

Participants

Reaction Steps

4.8 g (19.7 mmol) of 4-aminobenzilic acid was dissolved in 200 ml of absolute ethanol (EtOH) saturated with dry HCl gas. The reaction mixture was refluxed for 24 hours then spin evaporated to dryness in vacuum. The residue was dissolved in water and neutralized with NaHCO3, extracted with 2×50 ml of AcOEt, washed with water (2×) and the AcOEt extract filtered through a siliconized filter and dried over MgSO4. The dried solution was filtered and spin evaporated in vacuum. Yellow oil, 2.8 g (52%). SGTLC in acetone Rf 0.8. HPLC Bondapak μC18MeOH/H2O (75:25) pH 4 (formic acid). Elemental Analysis Calc. for C16H17NO3. Calc. C 70.83, H 6.32, N 5.16; Found C 70.77, H 6.47, N 5.04, 5.26.

Provenance & Evidence