Oxalic Acid → HCID 71185455, compound

Participants

Reaction Conditions

Reaction Steps

A solution containing (5a) (2.5 mmol) in toluene (15 ml) was injected over 1 hour through a 20 cm column packed with quartz tubes heated at 410° C. using argon as carrier. The column was washed with 5 ml of pure toluene and the collected mixture was evaporated to dryness. The concentrate was added to a solution of oxalic acid (1.12 mmol) in THF (10 ml) and water (1 ml) and the mixture was stirred at room temperature for 1 hour then quenched with a saturated bicarbonate solution and extracted with diethylether. The organic layer was washed with water and brine, then dried with MgSO4, and evaporated to dryness. The crude was purified by bulb-to-bulb distillation and column chromatography (Silicagel, Cyclohexane/EtOAc 99/1). Yield: 62%.

Provenance & Evidence