反应详情

温度

40 °C

Glutaric anhydride (11.41 g.) was added portion-wise to a solution of potassium tert-butoxide (14.02 g.) in tetrahydrofuran (100 ml.) at ambient temperature. After the exothermic reaction was ceased, the reaction mixture was stirred at 40° C. for 15 minutes. Tetrahydrofuran was distilled off under reduced pressure. The residue was dissolved in water. After ethyl acetate was added, the solution was adjusted to pH 9 with aqueous potassium carbonate solution under ice-cooling. The separated water layer was washed with ethyl acetate, treated with activated charcoal, overlapped with ethyl acetate, and then adjusted to pH 4.0 with 10% hydrochloric acid under ice-cooling. The ethyl acetate layer was dried over magnesium sulfate, treated with activated charcoal, filtered and concentrated under reduced pressure to give glutaric acid mono-tert-butyl ester (10 g.).

1. customAfter the exothermic reaction
2. distillationTetrahydrofuran was distilled off under reduced pressure
3. dissolutionThe residue was dissolved in water
4. additionAfter ethyl acetate was added
5. temperaturecooling
6. washThe separated water layer was washed with ethyl acetate
7. additiontreated with activated charcoal
8. temperaturecooling
9. dry with materialThe ethyl acetate layer was dried over magnesium sulfate
10. additiontreated with activated charcoal
11. filtrationfiltered
12. concentrationconcentrated under reduced pressure