Acetic Anhydride → HCID 178472731, compound

Participants

Reaction Steps

To a solution of compound F (6.6 g, 7.8 mmol) in CHCl3 (50 mL) at 5° C. was added DIPEA (4.8 mL, 27.4 mmol) followed by Ac2O (0.9 mL, 9.4 mmol). The reaction mixture was stirred at ambient temperature for 30 min. Solvents were removed in vacuo, and then the residue was diluted with water (500 mL) and EtOAc (500 mL). The organic layer was separated and washed with water (300 mL), 2% aqueous H2SO4 (200 mL), water (2×300 mL) and brine (100 mL). The organic layer was separated, dried over Na2SO4 and solvent removed in vacuo to afford compound G (5.5 g, 82%). LC-MS [M+H] 853.4 (C36H52N8O12S2+H, calc: 853.9). Purity >95% (UV/254 nm). Compound G was used without further purification.

Provenance & Evidence