Potassium Carbonate → HCID 21541521, compound

Participants

Reaction Steps

A mixture of VI (2.73 g, 0.00745 mole), methanol (100 ml), and 20% aqueous potassium carbonate solution (30 ml) was stirred and heated under reflux for 1 hour. The turbid solution was concentrated to 1/4 of the volume by distillation from a water bath (60°C) under reduced pressure (60 mm Hg). The residue was diluted with water (100 ml) and adjusted to pH 7 with acetic acid (2.7 ml). The resulting emulsion was extracted with two 80-ml portions of ether. The combined ethereal extracts were washed with water (100 ml) and then dried over magnesium sulfate. Ether was distilled off from a water bath (50°C), at last under 15 mm Hg. The yellow, oily residue (2.58 g) was purified by crystallization from petroleum ether (boiling below 50°C) (450 ml). 2.13 g (84%) of VIa were hereby obtained as almost white crystals with m.p. 43°-45°C.

Provenance & Evidence