Methanesulfonyl chloride → HCID 86659107, compound

Participants

Reaction Steps

Methanesulfonyl chloride (0.06 mL, 1.474 mmol) and DIEA (0.243 mL, 1.394 mmol) were added to a stirring solution of Intermediate 134 (330 mg, 0.697 mmol) at rt. The reaction was monitored by LC/MS and additional methanesulfonyl chloride (0.06 mL, 1.474 mmol) and DIEA (0.243 mL, 1.394 mmol) were added after 3 h. The resulting reaction mixture was stirred for an additional 1 h then quenched with satd. NaHCO3 (50 mL). The aqueous layer was extracted with CH2Cl2 (3×20 mL). The combined organic layers were washed with H2O (100 mL), brine (100 mL), dried over Na2SO4 (s), and concentrated to give the title compound (460 mg) as a yellow solid. The compound was used with no further purification. ES/MS calcd. for C26H26N3O7S2+ 556.1. Found m/z=556.1 (M+H)+.

Provenance & Evidence