反应详情

While stirring a mixture of 22.5 g of ethyl 2-(4-formylphenoxy)propionate ([α]D25 =+51.5°) and 60 g of toluene at room temperature, 22.8 g of 40% peracetic acid was dropwise added. After stirring at 20° to 30° C. for 2 hours and at 50° C. for 2 hours, 0.2 g of water was added, and the mixture was stirred for 2 hours. After cooling the reaction mixture to room temperature, 40 g of water was added. The aqueous layer was separated. The organic layer was washed with 40 g of water, followed by washing twice with 40 g of a 5% sodium hydrogen carbonate aqueous solution, then with 40 g of a 5% sodium hydrogen sulfite aqueous solution and further with 40 g of water. Then, the reaction mixture was concentrated by distilling off toluene under reduced pressure, and subjected to distillation under reduced pressure, whereby 16.5 g of (+)-ethyl 2-(4-hydroxyphenoxy)propionate was obtained as a colorless transparent liquid. The boiling point was from 130° to 140° C./1 mmHg.

1. stirringAfter stirring at 20° to 30° C. for 2 hours and at 50° C. for 2 hours
2. stirringthe mixture was stirred for 2 hours
3. customThe aqueous layer was separated
4. washThe organic layer was washed with 40 g of water
5. washby washing twice with 40 g of a 5% sodium hydrogen carbonate aqueous solution
6. concentrationThen, the reaction mixture was concentrated
7. distillationby distilling off toluene under reduced pressure
8. distillationsubjected to distillation under reduced pressure