反应详情

Compound 1-1 was stirred with TMSBr (0.41 mL, 3.2 mmol) and 2.7 mL of CH2Cl2 for 5 hours before concentrating in vacuo to afford compound 1-2 as an oil. The oil was redissolved in 2 to 3 mL of MeOH and re-concentrated, then triturated with acetonitrile and EtOAc to afford title compound 1-2 as a white powder. mp 210-215° C.; LRMS (API-ES) m/e for C16H12ClN2O3PS (M+H)+, calcd 378.77. found 379.4; Anal. Calcd for C16H12ClN2O3PS+1 HBr: C, 41.81; H, 2.85; N, 6.09. Found: C, 42.11; H, 2.66; N, 6.21.

1. concentrationbefore concentrating in vacuo