Diisopropylethylamine → HCID 89402084, compound

Participants

Reaction Steps

In a 50-mL round-bottomed flask Intermediate 2 (0.4 g, 1.1 mmol) and 3,3-difluoroazetidine hydrochloride (0.17 g, 1.3 mmol) was dissolved in dichloromethane (20 mL). Propylphosphonic anhydride (0.42 g, 1.3 mmol), DIPEA (0.28 g, 2.2 mmol) was added at room temperature and stirred reaction mixture for 30 min. The progress of the reaction was followed by TLC analysis on silica gel with 0.5% Methanol:dichloromethane as mobile phase and visualization with U.V light, reaction mixture was quenched into ice water slurry, filter it, compound was extracted in dichloromethane, dried over Na2SO4, filtered, and concentrated by rotary evaporation (28° C., 20 mmHg) to afford 0.5 g of a solid crude, The purification done by Flash chromatography and product elute at neat dichloromethane to afford pure compound 0.030 g yield (6.2%).

Provenance & Evidence