Ethyl Acetate → HCID 118123634, compound

Participants

Reaction Steps

In a 100-mL three-neck flask, 3.1 g of 4-methoxycinnamic acid and 14.0 g of ethyl acetate were placed to give a suspension. The suspension was combined with 2.2 g 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 completion of reaction, 6.1 g of ethyl acetate was distilled off together with unreacted thionyl chloride and an acidic gas at 60° C. under reduced pressure. After the concentration, the resulting mixture was combined with ethyl acetate in an amount equal to the distilled-off amount and yielded 19.2 g of a 4-methoxycinnamoyl chloride/ethyl acetate solution (3).

Provenance & Evidence