N-bromobutanimide → HCID 66968760, compound

Participants

Reaction Steps

A 25 mL round bottom flask under nitrogen was charged with the product of Example 82 Step 1 (238 mg, 0.438 mmol), NBS (39.0 mg, 0.219 mmol), and acetonitrile (15 ml). Stirred at room temperature 10 minutes. HPLC/MS shows mainly desired; little starting material. Added an additional 10 mg NBS. Still a little starting material remaining. Added another 10 mg NES. HPLC/MS looks good. Cooled. Evaporated. Subjected to ISCO chromatography eluting with a hexane/ethyl acetate gradient. Evaporated fractions containing product to give the title compound as a white solid. (224 mg, 0.360 mmol, 82% yield). LCMS (ES+) m/z 623.3 (M+H)+.

Provenance & Evidence