Ethanol → HCID 89656036, compound

Participants

Reaction Conditions

Reaction Steps

The product from Example 51A (3.24 g, 9.81 mmol), iron (2.74 g, 49.1 mmol), and ammonium chloride (0.787 g, 14.72 mmol) were combined in the solvent mixture of tetrahydrofuran (21.0 mL), ethanol (21.0 mL) and water (7.0 mL) and heated at 95° C. with vigorous stirring for 3 hours. The mixture was cooled and filtered through a plug of Celite to remove solids. The plug was rinsed repeatedly with methanol and tetrahydrofuran. The filtrate was concentrated and the residue partitioned between ethyl acetate and water. The organic layer was washed with saturated aqueous sodium chloride, dried (anhydrous Na2SO4), filtered, and concentrated to afford the title compound (2.81 g, 95%).

Provenance & Evidence