反应 #1923
ord-cca8c52f7ba34625b95aa6d245498aa5
反应方程式
1-acetamido-6,11-dihydrodibenz[b,e]oxepin-11-one
sodium bicarbonate
→
1-amino-6,11-dihydrodibenz[b,e]oxepin-11-one
收率 81.0%
反应条件
详细条件
See reaction.notes.procedure_details.
后处理
- 1温度was heated
- 2温度under reflux for 2 hours
- 3萃取followed by extraction with ethyl acetate (25 ml)
- 4洗涤The organic layer was washed with a saturated aqueous solution of sodium chloride
- 5干燥dried over anhydrous magnesium sulfate
- 6过滤After the drying agent was filtered off
- 7浓缩the organic layer was concentrated under reduced pressure
实验过程
In concentrated hydrochloric acid (10 ml), 1-acetamido-6,11-dihydrodibenz[b,e]oxepin-11-one obtained in Reference Example 3(0.25 g, 0.94 mmol) was heated under reflux for 2 hours. The reaction mixture was poured into a saturated aqueous solution of sodium bicarbonate, followed by extraction with ethyl acetate (25 ml). The organic layer was washed with a saturated aqueous solution of sodium chloride, and then dried over anhydrous magnesium sulfate. After the drying agent was filtered off, the organic layer was concentrated under reduced pressure to give 1-amino-6,11-dihydrodibenz[b,e]oxepin-11-one as a yellow solid (0.17 g, 81%).