反应详情

Ethyl 2-ethoxybenzoate (100 g, 128.7 mmol) and hydrazine hydrate (100%, 25 ml, 128.7 mmol) are dissolved in 200 ml of ethanol and heated under reflux for 5 hours. A further 12.5 ml (64.3 mmol) of hydrazine hydrate are added and the reaction mixture is heated under reflux for a further 7 hours. For working up, the reaction mixture is extensively concentrated and then stirred with 300 ml of cyclohexane at room temperature. After cooling to 0° C., the crystals are filtered off with suction, washed twice with 50 ml of cold cyclohexane each time and finally dried in a vacuum oven at 35° C. and 300 mbar overnight.

1. temperatureheated
2. temperatureunder reflux for 5 hours
3. temperaturethe reaction mixture is heated
4. temperatureunder reflux for a further 7 hours
5. concentrationthe reaction mixture is extensively concentrated
6. temperatureAfter cooling to 0° C.
7. filtrationthe crystals are filtered off with suction
8. washwashed twice with 50 ml of cold cyclohexane each time
9. customfinally dried in a vacuum oven at 35° C.
10. custom300 mbar overnight