反应详情

2-Fluoro-4-nitrobenzoic acid methyl ester (5 g, 25.11 mmol) and hydrazine hydrate (1.34 ml, 27.62 mmol) were dissolved in 250 ml of ethanol and heated under reflux for 11 h. A further 0.26 ml of hydrazine hydrate were added and heated under reflux for a further 6 h, and the mixture was concentrated and ethyl acetate and water were added. The precipitated residue was filtered off with suction and dried. Purification by preparative HPLC (PR18, acetonitrile/water 0.1% TFA) resulted in 1.39 g of product, M+H+: 180.05.

1. temperatureheated
2. temperatureunder reflux for 11 h
3. temperatureheated
4. temperatureunder reflux for a further 6 h
5. concentrationthe mixture was concentrated
6. additionethyl acetate and water were added
7. filtrationThe precipitated residue was filtered off with suction
8. customdried
9. customPurification by preparative HPLC (PR18, acetonitrile/water 0.1% TFA)