反应 #2460292
ord-bc8a5c16748542c89324f2e12269afa9
反应方程式
反应条件
后处理
- 1其他First, 2-(4-butoxyphenoxy)benzoic acid was prepared
- 2温度was heated
- 3温度at reflux for 5 h
- 4温度cooled
- 5萃取The precipitated product was extracted into diethyl ether
- 6其他The product was purified by extraction into 5% aqueous NaOH
- 7其他The precipitate was collected
- 8洗涤washed with water
- 9干燥dried in vacuo over CaSO4
实验过程
First, 2-(4-butoxyphenoxy)benzoic acid was prepared. A stirred mixture of 2-chlorobenzoic acid (10.0 g, 64 mmol), 4-butoxyphenol (12.7 g, 77 mmol), potassium carbonate (17.6 g, 128 mmol), copper powder (0.24 g, 3.8 mmol), copper (I) iodide (0.20 g, 1.3 mmol), dithioerithritol (0.20 g, 1.3 mmol), and 75 mL of N,N-dimethylformamide was heated at reflux for 5 h and then cooled to ambient. The reaction mixture was poured onto a mixture of 300 g of ice plus 100 mL of 10% aqueous HCl. The precipitated product was extracted into diethyl ether. The product was purified by extraction into 5% aqueous NaOH, followed by acidification with concentrated HCl. The precipitate was collected, washed with water, and dried in vacuo over CaSO4 to provide 8.27 g (45% of theory) of 2-(4-butoxyphenoxy)benzoic acid as a brown powder.