反应详情

温度

110 °C

The (2,2-difluoro-benzo[1,3]dioxol-4-yl)-hydrazine (753 mg, 4.00 mmol) and 4-piperidone hydrochloride (543 mg, 4.00 mmol) in ethanol (10 mL) were heated to reflux for 45 min. The 4M HCl in dioxane (2 mL) was added and heating continued for 2 h. A sample was removed and after bubbling HCl gas briefly was heated in the microwave to 110° C. for 10 min. The rest of the material was processed in 5 batches and the combined black reactions filtered, washed with a little water and then precipitation with Et2O:Hexane 1:2 (c.f. 10 mL) before drying the resulting grey solid (147 mg, 13% yield)

1. temperatureto reflux for 45 min
2. temperatureheating
3. customA sample was removed
4. customafter bubbling HCl gas
5. filtrationthe combined black reactions filtered
6. washwashed with a little water
7. customprecipitation with Et2O:Hexane 1:2 (c.f. 10 mL)