反応 #76448

反応方程式

hydrochloric acid

methyl 4-fluoro-3-nitrophenylacetate

hydrochloric acid

isopropanol

→

methyl 3-amino-4-fluorophenylacetate

収率 98.0%

溶媒

water

反応条件

後処理

1. 1
   温度the mixture was heated
2. 2
   温度to reflux for 1 hour
3. 3
   温度the mixture was refluxed for a further 1 hour
4. 4
   温度The mixture was cooled to room temperature
5. 5
   ろ過filtered through a plug of Hyflo® diatomaceous earth
6. 6
   その他the filtrate was evaporated in vacuo

実験手順

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.

出典