Potassium Hydroxide → HCID 69309430, compound

Participants

Reaction Conditions

Reaction Steps

19 g of ethyl hydroxycinnamate and 7.3 g of potassium hydroxide were added to 150 ml of ethanol, and stirred at 50° C. for 1 hour. This was cooled to 40° C., and 35 g of 3-[(tosyloxy)methyl]-3-ethyloxetane was dropwise added to it. Then, this was refluxed for 3 hours. Ethanol was evaporated away, and water and toluene were added to it for liquid-liquid separation. The toluene layer was washed with 3% hydrochloric acid, saturated sodium hydrogencarbonate and water, and then toluene was evaporated away. To the resulting residue, added were 20 g of sodium hydroxide, 100 ml of ethanol and 50 ml of water, and this was refluxed for 2 hours. Ethanol was evaporated away, and the resulting residue was poured into 500 ml of 5% hydrochloric acid, and a crystal was thus formed. The crystal taken out through filtration was recrystallized from a mixed solvent of ethanol and water, and 5 g of 4-(3-ethyloxetan-3-ylmethoxy)cinnamic acid (OX6) was obtained. Its melting point was 127.5° C.

Provenance & Evidence