反应详情

A suspension of 50 g. (0.155 mole) of 3-phenyl-5-(β-hydroxyphenethyl)-N-methyl-isoxazole-4-carboxamide and 800 ml. acetic acid at room temperature is treated dropwise rapidly with 18.4 g. (0.185 mole) of chromium trioxide in 185 ml. water. The resulting solution is stirred for 2 hours at room temperature and a portion of the acetic acid is removed in vacuo. The remainder is poured onto ice water and extracted with methylene chloride. The methylene chloride layer is washed with 2 N sodium hydroxide, dried over anhydrous magnesium sulfate, filtered and evaporated in vacuo. The solid residue is triturated with hot ether, cooled to 0° C. and filtered to give N-methyl-5-phenacyl-3-phenyl-4-isoxazole carboxamide, m.p. 125° to 128° C.

1. additionA suspension of 50 g
2. customa portion of the acetic acid is removed in vacuo
3. additionThe remainder is poured onto ice water
4. extractionextracted with methylene chloride
5. washThe methylene chloride layer is washed with 2 N sodium hydroxide
6. dry with materialdried over anhydrous magnesium sulfate
7. filtrationfiltered
8. customevaporated in vacuo
9. customThe solid residue is triturated with hot ether
10. temperaturecooled to 0° C.
11. filtrationfiltered