Hydrochloric Acid → HCID 54018478, compound

Participants

Reaction Steps

5-methoxy-2-methyl-1-(ρ-methylsulfonylbenzylidene)-3-indenyl acetic acid is prepared by the dissolving 0.03 moles of the sulfoxide in 25 ml. methanol, and 50 ml. acetonitrile are added. The solution is stirred at 0 C., and 0.03 moles of sodium methoxide are added dropwise. Stirring is continued, and 0.06 mole sodium bicarbonate is added as well a 0.06 moles of H2O2 (30% solution in water). The temperature is then dropped to -10 C., and stirring continued for 30 hours. At this time the NaHCO3 is filtered and washed on the filter with a few ml. of cold methanol. The washings are returned to the filtrate and the NaHCO3 is discarded. The filtrate is neutralized with 0.07 moles of HCl (concentrated HCl), partially evaporated to 50% of the original volume, and returned to the freezer for crystallization. Crystals of the sulfone derivative are collected. Additional sulfone can be collected from the mother liquor in a similar manner. (R1 =hydrogen; R2 =CH3 ; R3 =5--OCH3 ; R4 =hydrogen; R5 =p--CH3SO2)

Provenance & Evidence