反应详情

Iron powder (8.1 g) was added to a solution of methyl 4-fluoro-3-nitrophenylacetate (27.24 g, 0.128 mol) in a mixture of concentrated hydrochloric acid (1.5 ml), isopropanol (265 ml) and water (26.5 ml) and the mixture was stirred at room temperature for 1 hour. A second portion of iron powder (8.1 g) was added and the mixture was heated to reflux for 1 hour. A further quantity of concentrated hydrochloric acid was added and the mixture was refluxed for a further 1 hour. The mixture was cooled to room temperature, filtered through a plug of Hyflo® diatomaceous earth and the filtrate was evaporated in vacuo to give methyl 3-amino-4-fluorophenylacetate (22.98 g) which was used without further purification in the next step.

1. temperaturethe mixture was heated
2. temperatureto reflux for 1 hour
3. temperaturethe mixture was refluxed for a further 1 hour
4. temperatureThe mixture was cooled to room temperature
5. filtrationfiltered through a plug of Hyflo® diatomaceous earth
6. customthe filtrate was evaporated in vacuo