Methacrylic Acid → HCID 57679346, compound

Participants

Reaction Conditions

Reaction Steps

A solution of 66.9 g of benzo[b]thiophene (0.5 mol) and 46.3 g of methacrylic acid (0.537 mol) in 60 ml of dichloromethane was added dropwise starting at 70° C. within 20 minutes to 1000 g of super-PPA. The temperature was maintained at 65-70° C. during the addition. Methylene chloride was distilled off. After 2 h of reaction time, the reaction mixture was poured onto crushed ice and stirred until the polyphosphoric acid had completely dissolved. The aqueous phase was extracted with a dichloromethane/hexane solvent mixture (30 parts by volume/70 parts by volume). The combined organic phases were washed with a saturated aqueous solution of sodium hydrogen-carbonate and with water and dried over magnesium sulfate. After removing the solvents under reduced pressure, 79.8 g of a dark orange oil (71%) were obtained.

Provenance & Evidence