Ethyl Acetate → HCID 118123634, compound

Participants

Reaction Steps

In a 1.5-m3 reactor, 105 kg of 4-methoxycinnamic acid and 462 kg of ethyl acetate were placed to give a suspension. The suspension was combined with 73.6 kg of thionyl chloride (1.05 times the mole of 4-methoxycinnamic acid) added dropwise while maintaining the reactor inside temperature at 65° C. to 70° C. After the dropwise addition, a reaction was performed until the conversion from 4-methoxycinnamic acid reached 99% or more. After the completion of reaction, about 200 kg of ethyl acetate was distilled off together with unreacted thionyl chloride and an acidic gas at 60° C. under reduced pressure. After the concentration by distillation, the mixture was combined with ethyl acetate in an amount equal to the distilled-off amount and yielded 579.6 kg of a 4-methoxycinnamoyl chloride/ethyl acetate solution (1).

Provenance & Evidence