反应详情

温度

20 °C

(3-Phenoxyphenyl)acetic acid (11.5 g) and 36N aqueous sulphuric acid solution (3 cc) in ethanol (200 cc) are brought to boiling for 72 hours. After being cooled to approximately 20° C., the reaction mixture is concentrated to dryness at 50° C. under reduced pressure (20 mm Hg; 2.7 kPa). The oil is dissolved in dichloromethane (300 cc); the organic phase is washed with water (150 cc), dried over anhydrous magnesium sulphate, filtered and concentrated to dryness at 40° C. under reduced pressure (20 mm Hg; 2.7 kPa). The residue is dissolved in a mixture (20 cc) of cyclohexane and ethyl acetate (50:50 by volume), and the solution is poured onto silica (400 g) contained in a column 5 cm in diameter. Elution is performed with a mixture of cyclohexane and ethyl acetate (50:50 by volume), and the corresponding eluate is concentrated to dryness at 40° C. under reduced pressure (20 mm Hg; 2.7 kPa). Ethyl (3-phenoxyphenyl)acetate (7.4 g) is thereby obtained, and is used in the crude state in the subsequent syntheses.

1. concentrationthe reaction mixture is concentrated to dryness at 50° C. under reduced pressure (20 mm Hg; 2.7 kPa)
2. dissolutionThe oil is dissolved in dichloromethane (300 cc)
3. washthe organic phase is washed with water (150 cc)
4. dry with materialdried over anhydrous magnesium sulphate
5. filtrationfiltered
6. concentrationconcentrated to dryness at 40° C. under reduced pressure (20 mm Hg; 2.7 kPa)
7. dissolutionThe residue is dissolved in a mixture (20 cc) of cyclohexane and ethyl acetate (50:50 by volume)
8. additionthe solution is poured onto silica (400 g)
9. washElution
10. additionis performed with a mixture of cyclohexane and ethyl acetate (50:50 by volume)
11. concentrationthe corresponding eluate is concentrated to dryness at 40° C. under reduced pressure (20 mm Hg; 2.7 kPa)