反应详情

温度

60 °C

12 g of ethyl hydroxybiphenylcarboxylate and 15 g of potassium hydroxide were added to 100 mL of ethanol, and stirred at 60° C. for 1 hour. After decreasing the temperature to 45° C., 15 g of 3-((tosyloxy)methyl)-3-ethyloxetane was added dropwise thereto, and then refluxed for 2 hours. Water and toluene were added thereto, and the toluene layer was separated. The toluene layer was washed with 3% hydrochloric acid, a saturated sodium carbonate solution and water, and then toluene was distilled off. 20 g of sodium hydroxide, 500 mL of ethanol and 100 mL of water were added to the resulting residue, and refluxed for 2 hours. A residue obtained by distilling ethanol off was put in 300 mL of 5% hydrochloric acid to obtain crystals. The crystals thus obtained by filtering were recrystallized from ethanol to obtain 8 g of 4-(3-ethyloxetane-3-ylmethoxy)biphenylcarboxylic acid (OX2), which had a melting point of 222 to 225° C.

1. customto 45° C.
2. temperaturerefluxed for 2 hours
3. customthe toluene layer was separated
4. washThe toluene layer was washed with 3% hydrochloric acid
5. distillationa saturated sodium carbonate solution and water, and then toluene was distilled off
6. addition20 g of sodium hydroxide, 500 mL of ethanol and 100 mL of water were added to the resulting residue
7. temperaturerefluxed for 2 hours
8. customA residue obtained
9. distillationby distilling ethanol
10. customto obtain crystals
11. customThe crystals thus obtained
12. filtrationby filtering
13. customwere recrystallized from ethanol