Phosphoric Acid → HCID 66920177, compound

Participants

Reaction Steps

The compound of step 2 (3.09 g, 11.0 mmol) was dissolved in DCM (83 ml), and N-chlorosuccinimide (1.54 g, 11.6 mmol) was added. The reaction mixture was stirred at room temperature for 2 h. The solvent was removed, the resulting solid was dissolved in concentrated acetic acid (45 ml) and heated to 70° C. After the addition of phosphoric acid (9.35 ml, 137 mmol; 85%), the reaction mixture was heated to 120° C. for 2 h. The cooled mixture was diluted with water, extracted with EA, the organic layer separated, dried over sodium sulfate, filtered, and evaporated. The residue was purified by silica gel chromatography (EA/HEP 1:6). 2.38 g of the title compound was obtained.

Provenance & Evidence