反应详情

Ethyl 2-[4-(2,2-dimethoxyethyl)-2,5-dimethylphenoxy]acetate (43 g) was dissolved in acetonitrile (190 g) while stirring. To the resulting solution was added 10% perchloric acid (216 g), and the mixture was stirred for an hour at room temperature. The reaction mixture was partitioned between toluene (340 g) and water (200 g). The organic layer was washed with water, an aqueous solution of sodium bicarbonate and brine successively, and dried over anhydrous sodium sulfate, followed by concentration under reduced pressure. The residue was dissolved in ethanol (180 g), and the solvent was removed under reduced pressure. The residue was dissolved with hexane (86 g) and ethanol (37 g). After seed crystals were added, the solution was stirred at 0-10° C. for 2 hours. Hexane (220 g) was added, and the resulting suspension was stirred at 0-10° C. for 2 hours. The precipitated crystals were filtered to give ethyl 2-[4-(2-ethoxy-2-hydroxyethyl)-2,5-dimethylphenoxy]acetate (21 g).

1. stirringthe mixture was stirred for an hour at room temperature
2. customThe reaction mixture was partitioned between toluene (340 g) and water (200 g)
3. washThe organic layer was washed with water
4. dry with materialan aqueous solution of sodium bicarbonate and brine successively, and dried over anhydrous sodium sulfate
5. concentrationfollowed by concentration under reduced pressure
6. dissolutionThe residue was dissolved in ethanol (180 g)
7. customthe solvent was removed under reduced pressure
8. dissolutionThe residue was dissolved with hexane (86 g) and ethanol (37 g)
9. additionAfter seed crystals were added
10. stirringthe solution was stirred at 0-10° C. for 2 hours
11. additionHexane (220 g) was added
12. stirringthe resulting suspension was stirred at 0-10° C. for 2 hours
13. filtrationThe precipitated crystals were filtered