1620
F. Shirini et al.
Chlorosulfonic acid (23.3 g, 0.2 mmol) was added dropwise over a pe-
riod of 30 min at room temperature. HCl gas evolved from the reaction
vessel immediately (Scheme 1). After the addition was complete the
mixture was shaken 30 min. A white solid (silica sulfuric acid, 76.0 g)
was obtained.
General Procedure for Acetylation and Formylation of Alcohols in the
Presence of Silica Sulfuric Acid. A mixture of the substrate (1 mmol),
acid (1 mmol), and silica sulfuric acid (0.05 g) in n-hexane (3 mL) was
refluxed for the specified time (Table I). The reaction was monitored by
TLC or GC. After completion of the reaction, the mixture was filtered
and the solid residue was washed with dichloromethane (10 mL). Evap-
oration of the solvent followed by column chromatography on silica gel
gave the corresponding esters in good to high yields.
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