反应详情

A suspension of 145 mg (0.5 mmol) of Compound 17, 104 mg (1.5 mmol) of hydroxylamine hydrochloride and 123 mg (1.5 mmol) of -sodium acetate in 15 ml of methanol was refluxed for 166 hours. The reaction mixture was concentrated under reduced pressure, followed by the addition of a half-saturated aqueous solution of potassium carbonate to the residue. The resulting mixture was extracted with chloroform (twice). The organic layer was washed with a saturated aqueous solution of sodium chloride, dried over anhydrous sodium sulfate, and then concentrated under reduced pressure. The residue was purified by chromatography on a silica gel column (eluent: chloroform), whereby 69 mg of the title compound were obtained (yield: 45%).

1. temperaturewas refluxed for 166 hours
2. concentrationThe reaction mixture was concentrated under reduced pressure
3. additionfollowed by the addition of a half-saturated aqueous solution of potassium carbonate to the residue
4. extractionThe resulting mixture was extracted with chloroform (twice)
5. washThe organic layer was washed with a saturated aqueous solution of sodium chloride
6. dry with materialdried over anhydrous sodium sulfate
7. concentrationconcentrated under reduced pressure
8. customThe residue was purified by chromatography on a silica gel column (eluent: chloroform)