Phosphorus oxychloride → HCID 19903221, compound

Participants

Reaction Steps

Phosphorus oxychloride (22 mL) was added with stirring to DMF (220 mL). The exothermic reaction mixture turned deep red, and compound VI (23.20 g, 85 mmol) was added. The mixture was cooled in a water bath and stirred for 20 hr. The DMF was then removed under vacuum and the residue was dissolved in methylene chloride (300 mL). Saturated aqueous sodium carbonate (ca 200 mL) was added to the solution with ice bath cooling until no more bubbling was observed. The methylene chloride layer was separated and concentrated in vacuo. The residue was recrystallized from hexanes-ethyl acetate to give the crystalline product (19.0 g, 87%).

Provenance & Evidence