a ph of 1 to 2 with concentrated hydrochloric acid the 4 methoxyphenol was extracted with three 100 ml portions of methylene chloride the organic solution containing the neutrals as well as the one containing the product were separately dried over anhydrous magnesium sulfate and filtered into tared round bottom flasks the methylene chloride was removed using a rotary evaporator a total of 0 052 g of neutrals was recovered a total of 4 13 g of the crude 4 methoxyphenol was obtained 33 3 mmol 90 7 yield the 4 methoxyphenol was purified utilizing bulb to bulb distillation a mass of 3 88 g of 4 methoxyphenol as a white crystalline solid was obtained 31 3 mmol 85 1 yield the purity was determined by gc 99 7 as well as hplc 99 3 in a 500 ml flask were placed 5 0 g 30 1 mmol of 2 3 dimethoxybenzaldehyde and 150 ml of methylene chloride 0 2m this mixture was vigorously stirred with a magnetic stir bar to the homogeneous solution was added 7 68 ml of 30 aqueous hydrogen peroxide 75 0 mmol 2 5 equivalents and 5 54 ml of formic acid 120 0 mmol 4.