Acetic Anhydride → HCID 67246495, compound

Participants

Reaction Steps

Perchloric acid (70% aq.; 1.0 ml) was added slowly to freshly distilled Ac2O (25 ml) at 0° C. The compound of example 20a (31.8 g; 125 mmol) in CH2Cl2 (13 ml) was added drop wise at 10-15° C. The reaction mixture was heated on steam bath for 1 h, concentrated, poured over crushed ice and NaHCO3 (˜25 g) and extracted with ether. The ether layer was washed with brine, dried (Na2SO4), concentrated and purified using flash chromatography (silica gel, 5% CH3CN in CHCl3) to obtain the title compound. Yield, 24.6 g (61.5%), semisolid; analysis: C16H20O7: requires C, 59.25; H, 6.22. found: C, 59.57; H, 6.28%.

Provenance & Evidence