反应详情

A mixture of 1,2,3,4-tetrahydro-benzo[b]azepin-5-one (5) (1.58 g, 9.80 mmol), hydrazine monohydrate (1.92 mL, 40.0 mmol), and KOH (3.3 g, 58.8 mmol) in diethylene glycol (50 mL) was heated to reflux for 6 hr under a N2 atmosphere. After cooling, the reaction was poured onto ice-cold water, neutralized with 1N HCl, and extracted with EtOAc. All the organics were washed with water and saturated NaCl. Dried over MgSO4, filtered, and concentrated to yield compound 6 (0.69 g). This crude material was used in the next step with out further purification.

1. temperaturewas heated
2. temperatureto reflux for 6 hr under a N2 atmosphere
3. temperatureAfter cooling
4. additionthe reaction was poured onto ice-cold water
5. extractionextracted with EtOAc
6. washAll the organics were washed with water and saturated NaCl
7. dry with materialDried over MgSO4
8. filtrationfiltered
9. concentrationconcentrated