反应详情

温度

0 °C

A solution of 3,5-Di-tert-butyl-4-hydroxy-benzaldehyde oxime (3.0 grams, 8.4 mmole) in acetic anhydride (6 ml) was was refluxed for 2 hours. The mixture was cooled to 0° C. and saturated sodium hydrogencarbonate was added. The mixture was extracted with methylene chloride. The combined extracts were washed with saturated NaHCO3, dried over Na2SO4, filtered, and concentrated to give a solid. This was dissolved in diethyl ether and extracted with 1 N sodium hydroxide which was then acidified to pH 1 and extracted with ethyl acetate. The extract was dried and concentrated to a yellow solid which was recrystalized from ethyl acetate/hexane to give white crystals (1.05 g). MW 231; MS (m/e) 249 (M++NH4+).

1. extractionThe mixture was extracted with methylene chloride
2. washThe combined extracts were washed with saturated NaHCO3
3. dry with materialdried over Na2SO4
4. filtrationfiltered
5. concentrationconcentrated
6. customto give a solid
7. extractionextracted with 1 N sodium hydroxide which
8. extractionextracted with ethyl acetate
9. customThe extract was dried
10. concentrationconcentrated to a yellow solid which
11. customwas recrystalized from ethyl acetate/hexane