反应详情

To a solution of 3.78 g of p-acetamidophenol, 1.1 g of sodium methoxide, and 50 mg of potassium iodide in 40 ml of methanol is added 7.11 g of methyl α-bromo-α-[p-(p-chlorophenoxy)phenyl]acetate in 15 ml of benzene. The mixture is refluxed for 20 hours, poured into ice and water and extracted with chloroform. The chloroform extracts are washed with 10% potassium carbonate and with water. The extract is dried over magnesium sulfate and concentrated to a gum under vacuum. Petroleum ether is added to the residue and several ml of acetone. Scratching the flask gives crystals which are filtered to give the product as pink crystals, mp 152°-157° C. The crystals are dissolved in a minimum amount of hot acetone, the solution chilled and diluted with petroleum ether. Chilling and filtering gives pale pink crystals mp 157°-160° C.

1. temperatureThe mixture is refluxed for 20 hours
2. extractionextracted with chloroform
3. washThe chloroform extracts are washed with 10% potassium carbonate and with water
4. dry with materialThe extract is dried over magnesium sulfate
5. concentrationconcentrated to a gum under vacuum
6. additionPetroleum ether is added to the residue and several ml of acetone
7. customgives crystals which
8. filtrationare filtered