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- General Procedure: A mixture of dithioacetal of p-methoxy benzaldehyde (212 mg, 1 mmol), FeCl3 (162 mg, 1 mmol) and KI (166 mg, 1 mmol) was refluxed in methanol. Progress of the reaction was monitored by TLC. After the completion of the reaction, methanol was removed under reduced pressure and residue was extracted in ether. The ether extract was dried over anhydrous Na2SO4 and the organic layer was filtered. Evaporation of the solvent under reduced pressure furnished pure anisaldehyde (122 mg, 90%). IR (film, cm−1) : ν = 3009, 2739, 1684, 1578, 1511, 1461. 1H NMR (CDCl3, 200 MHz): δ = 3.89 (s, 3H), 7.01 (d, J = 8.7 Hz, 2H), 7.85 (d, J = 8.7 Hz, 2H), 9.90 (s, 1H). 13C NMR (CDCl3, 50 MHz): δ = 190.6, 164.4, 131.7, 129.7, 114.1, 55.3