反应详情

温度

23 °C

To a solution of 35.72 g (0.893 mol) sodium hydroxide in 357 ml water was added 100 g (0.893 mol) 3-fluorophenol. The reaction was heated to reflux and to the gently refluxing solution was added 72.8 ml (0.893 mol) beta-butyrolactone dropwise over 1.5 hours. The reaction was cooled to 23° C. and the pH brought to 2 with concentrated hydrochloric acid. The reaction was extracted with 300 ml diethyl ether and the ether layer was separated, washed with brine and then extracted with 3×200 ml saturated sodium bicarbonate. The combined bicarbonate layers were washed with 200 ml diethyl ether, acidified with 50 ml concentrated hydrochloric acid and extracted with 300 ml diethyl ether. The latter ether extract was washed with brine, dried over magnesium sulfate and concentrated in vacuo to give the product as a red oil, 31.6 g (17.9%).

1. temperatureThe reaction was heated
2. temperatureto reflux and to the gently refluxing solution
3. extractionThe reaction was extracted with 300 ml diethyl ether
4. customthe ether layer was separated
5. washwashed with brine
6. extractionextracted with 3×200 ml saturated sodium bicarbonate
7. washThe combined bicarbonate layers were washed with 200 ml diethyl ether
8. extractionextracted with 300 ml diethyl ether
9. extractionThe latter ether extract
10. washwas washed with brine
11. dry with materialdried over magnesium sulfate
12. concentrationconcentrated in vacuo