Dimethylformamide → HCID 85906589, compound

Participants

Reaction Steps

A solution of DMF (2.1 ml) and DCM (2.1 ml) was cooled to 0° C. and stirred under argon. Within 15 min phosphorus oxychloride (2.1 ml, 22.6 mmol) was added and the reaction mixture was stirred for 30 min at 0° C. The compound of step 1 (550 mg, 2.30 mmol), dissolved in chloroform (5.27 ml) and pyridine (1.05 ml), was then added to the cooled solution. The reaction mixture was stirred at room temperature overnight. The mixture was slowly poured into 300 ml of ice, and after a few minutes EA was added. The organic layer was separated, dried over sodium sulfate, filtered and evaporated under reduced pressure. Column chromatography on silica gel (EA/HEP 1:4) yielded 369 mg of the title compound as a white solid.

Provenance & Evidence