反応 #43586

反応方程式

3-fluoro-4,5-dihydroxybenzaldehyde

potassium carbonate

1,2-dibromoethane

→

desired compound

収率 95.4%

8-fluoro-2,3-dihydro-1,4-benzodioxin-6-carboxaldehyde

収率 95.4%

溶媒

DMF

反応条件

後処理

1. 1
   その他was removed under reduced pressure
2. 2
   workup.ADDITIONThe reaction mixture was then treated with dichloromethane and water
3. 3
   抽出The aqueous phase was extracted twice with dichloromethane
4. 4
   その他the combined organic phases were dried
5. 5
   その他the solvent was removed under reduced pressure

実験手順

To a solution of 3-fluoro-4,5-dihydroxybenzaldehyde (0.66 g, 4.2 mmol) in DMF (30 ml) was added potassium carbonate (1.15 g, 8.3 mmol) and 1,2-dibromoethane (0.72 ml, 8.3 mmol) and the resultant mixture was heated to 80° C. for 18 h before the solvent was removed under reduced pressure. The reaction mixture was then treated with dichloromethane and water. The aqueous phase was extracted twice with dichloromethane and the combined organic phases were dried and the solvent was removed under reduced pressure to give the desired compound as a cream solid (0.73 g, 95%).

出典