反应详情

To a solution of methyl 4-(2-fluoroethoxy)benzoate (7.7 g, 38.85 mmol) in dioxane (100 mL) was added LiOH (2M, 39 mL). The reaction mixture was stirred at room temperature for 18 hours, and then concentrated in vacuo. The residue was dissolved in H2O (30 ml) and extracted with ether. Under cooling the aqueous was acidified with HCl (6N) and extracted with CHCl3. The organic extracts were dried over MgSO4. Evaporation and recrystallization from ethyl acetate and methylene chloride gave the title compound as a white solid (5 g, 71% yield); 1H NMR (400 MHz, DMSO-d6) δ 4.28 (m, 1H), 4.35 (m, 1H,) 4.68 (m, 1H), 4.80 (m, 1H), 7.04 (d, 2H), 7.89 (d, 2H); MS m/e (M−H)− 183.1; mp 203° C.

1. concentrationconcentrated in vacuo
2. dissolutionThe residue was dissolved in H2O (30 ml)
3. extractionextracted with ether
4. temperatureUnder cooling the
5. extractionextracted with CHCl3
6. dry with materialThe organic extracts were dried over MgSO4
7. customEvaporation and recrystallization from ethyl acetate and methylene chloride