反应详情

To N,N-dimethylformamide (81 g) were added 4-(1-hydroxy-2,2-dimethoxyethyl)-2,5-dimethylphenol (20.0 g), potassium carbonate (15.8 g) and ethyl chloroacetate (12.4 g) at room temperature with stirring. The mixture was stirred at room temperature for an hour, and then stirred at 71° C. for 2 hours. The reaction mixture was diluted with ethyl acetate, washed with water and brine, and dried over anhydrous sodium sulfate. The organic layer was concentrated under reduced pressure, and a mixture of ethyl acetate and hexane was added to the residue. The precipitated crystals were collected by filtration to give ethyl 2-[4-(1-hydroxy-2,2-dimethoxyethyl)-2,5-dimethyl-phenoxy]acetate (21.3 g).

1. stirringThe mixture was stirred at room temperature for an hour
2. stirringstirred at 71° C. for 2 hours
3. washwashed with water and brine
4. dry with materialdried over anhydrous sodium sulfate
5. concentrationThe organic layer was concentrated under reduced pressure
6. additiona mixture of ethyl acetate and hexane
7. additionwas added to the residue
8. filtrationThe precipitated crystals were collected by filtration