反应详情

To mechanically stirred conc. H2SO4 (700 mL) at 3° C. was added p-hydroxyacetophenone (66.0 g, 480 mmol) followed by KNO3 (48.3 g, 477 mmol) in two approximately equal portions about four minutes apart. An additional 3.76 g of KNO3 was added after 1.67 hours to insure reaction completion. The reaction was slowly poured into 8 L crushed ice/water and extracted with 4 L ethyl acetate (EtOAc). The extract was concentrated in vacuo to a volume of ~1.25 L, 500 mL heptane were added and concentration was continued. Once a thick yellow suspension formed at 50° C., it was cooled to ~10° C. and filtered. The collected solids were washed with ~150 mL heptane and dried in vacuo at ~40° C. to give 81.8 g of the title compound.

1. customreaction completion
2. additionThe reaction was slowly poured into 8 L
3. extractionextracted with 4 L ethyl acetate (EtOAc)
4. concentrationThe extract was concentrated in vacuo to a volume of ~1.25 L, 500 mL heptane
5. additionwere added
6. concentrationconcentration
7. customOnce a thick yellow suspension formed at 50° C.
8. temperatureit was cooled to ~10° C.
9. filtrationfiltered
10. washThe collected solids were washed with ~150 mL heptane
11. customdried in vacuo at ~40° C.