Sodium Carbonate → HCID 86615560, compound

Participants

Reaction Steps

A suspension of the product of Example 202B (414 mg, 0.9153 mmol) and iron powder (204.5 mg, 3.66 mmol) in acetic acid (7 mL) and ethanol (7 mL) was heated at reflux under a nitrogen atmosphere for 1 hour. The reaction was cooled to room temperature, and the mixture was diluted with water (50 mL) and ethyl acetate (100 mL). The aqueous pH was adjusted to 5 with solid sodium carbonate, the layers were separated, and the organic phase washed with water (2×50 mL) and brine (50 mL). The organic extract was dried over sodium sulfate, filtered, and concentrated under vacuum to provide the title compound as a yellow solid (315 mg, 90%).

Provenance & Evidence