Methanesulfonyl chloride → HCID 68194838, compound

Participants

Reaction Steps

To a solution of Example 109B (75 mg, 0.149 mmol) in 2 mL N,N-dimethylformamide was added diisopropylethylamine (0.130 ml, 0.744 mmol) followed by methanesulfonyl chloride (0.017 ml, 0.223 mmol). The reaction mixture was stirred at room temperature overnight, then diluted with ethyl acetate. The organics were washed with saturated aqueous NaHCO3, water, and brine, dried over MgSO4, filtered, and concentrated. The crude material was triturated with ethyl acetate, filtered and dried over high vacuum to provide the title compound. 1H NMR (300 MHz, DMSO-d6) δ 0.85-1.12 (m, 4H) 1.99 (s, 2H) 2.86-3.02 (m, 3H) 4.55 (s, 2H) 6.90 (d, J=8.33 Hz, 1H) 7.13 (d, J=1.59 Hz, 1H) 7.44-7.94 (m, 6H) 9.16 (s, 1H) 10.84 (s, 1H). MS (ESI+) m/z 582.1 (M+H)+.

Provenance & Evidence