反应详情

After 5.45 g of 1-(9,9-di-n-butylfluorene-2-yl)-ethanone (12) (17 mmol) was dispersed in 50 ml of ethanol and 1.42 g of hydroxylamine hydrochloride (20.4 mmol) and 1.67 g of sodium acetate (20.4 mmol) were added thereto, the reaction mixture was slowly heated and refluxed for 1 hour. The reaction mixture was cooled to room temperature, and 100 ml of distilled water was added thereto and stirred for about 30 minutes. Then, the product was extracted with 200 ml of ethylacetate and sequentially washed with saturated aqueous sodium bicarbonate solution and 100 ml of distilled water, and the recovered organic layer was dried over anhydrous magnesium sulfate, followed by distilling the solvent under reduced pressure. The obtained solid product was dried, thereby obtaining 4.97 g of 1-(9,9-di-n-butylfluorene-2-yl)-ethanone oxime (13) (87.3%) as a light yellow product.

1. temperaturethe reaction mixture was slowly heated
2. temperaturerefluxed for 1 hour
3. extractionThen, the product was extracted with 200 ml of ethylacetate
4. washsequentially washed with saturated aqueous sodium bicarbonate solution and 100 ml of distilled water
5. dry with materialthe recovered organic layer was dried over anhydrous magnesium sulfate
6. distillationby distilling the solvent under reduced pressure
7. customThe obtained solid product was dried