Dimethylformamide → HCID 19738008, compound

Participants

Reaction Steps

To a solution of the product from Step C. (2.75 g, 13.4 mmol) in anhydrous DMF (40 mL) cooled to 0° C. was added sodium hydride (60% dispersion in mineral oil, 1.18 g, 29.5 mmol), followed by methyl iodide (2.5 mL, 40.2 mmol). The reaction mixture stirred at ambient temperature for 4 h and was poured onto ice and extracted with ethyl acetate (3×80 mL). Evaporation gave 3.35 g of an orange liquid which was chromatographed (silica, eluting with 50% ethyl acetate-hexane) to give the desired product (2.42 g, 77%): mp 61°-63° C.

Provenance & Evidence