反应详情

温度

90 °C

276.6 g of 4-chlorobutyl acetate (1.8 mol) were added to a solution of 249 g of ethyl 4-hydroxybenzoate (1.5 mol), 3 g of potassium iodide (0.018 mol) and 248 g of potassium carbonate (1.8 mol) in 21 of DMF, and the mixture was stirred at 90° C. for 11 hours. The reaction mixture was poured into 5 l of ice-water, and the precipitate was filtered off with suction and washed with 41 of ice-water. The crude product was dissolved in 3 l of ethanol, potassium hydroxide (400 g) was added, and the mixture was refluxed for 3 hours. The reaction mixture was poured into 6 l of ice-water and acidified using concentrated hydrochloric acid, and the precipitate was filtered off. The precipitate was washed with water until neutral and subsequently dried, giving 282.1 g of 4-(4′-hydroxybutoxy)benzoic acid (yield 89%).

1. filtrationthe precipitate was filtered off with suction
2. washwashed with 41 of ice-water
3. dissolutionThe crude product was dissolved in 3 l of ethanol
4. additionpotassium hydroxide (400 g) was added
5. temperaturethe mixture was refluxed for 3 hours
6. additionThe reaction mixture was poured into 6 l of ice-water
7. filtrationthe precipitate was filtered off
8. washThe precipitate was washed with water until neutral and
9. customsubsequently dried