Acetic Anhydride → HCID 59467892, compound

Participants

Reaction Steps

To a 0° C. solution of compound 41 (0.41 g, 1.20 mmol) in dry CH2Cl2 (20 mL) were added Ac2O (1.12 mL, 12.0 mmol) followed by dropwise addition of Et3N (1.12 mL, 8.00 mmol), and DMAP (10 mg) The reaction was stirred for 18 h under N2 at room temperature. The reaction mixture was diluted with CH2Cl2 (20 mL), washed with saturated NaHCO3 (10 mL), water (2×10 mL), and saturated NaCl (2×10 mL). Dried over MgSO4 and filtered. The solvent was removed under reduced pressure and the product was purified by column chromatography (CH2Cl2/EtOAc 1:1), and triturated from CH2Cl2/hexanes to afford 48 as a yellow solid (0.24 g, 52%); MS m/z: 384 (M+H)+. Anal. Calcd. For, C19H17N3O2S2.0.1H2O: C, 59.23; H, 4.92; N, 10.91; S, 16.64. Found: C, 58.84; H, 4.55; N, 10.55; S, 16.32.

Provenance & Evidence