反応 #1144532
ord-366e6e684c544a08bf8344d4e24ece50
反応方程式
反応条件
温度
60°CELSIUS
詳細条件
See reaction.notes.procedure_details.
後処理
- 1抽出After extraction with ethyl acetate
- 2洗浄the organic layer was washed with water
- 3乾燥brine, dried (MgSO4)
- 4その他the solvent evaporated
- 5ろ過The solid was filtered off
- 6洗浄washed with hexane
- 7その他dried under vacuum
実験手順
The starting material 5-benzyloxy-2-fluoro-4-methylnitrobenzene was obtained by adding benzyl bromide (3 ml, 25 mmol) to a solution of 2-fluoro-5-hydroxy-4-methylnitrobenzene (3.92 mg, 23 mmol) in DMF (70 ml) containing potassium carbonate (9.5 g, 68 mmol). After stirring for 3 hours at 60° C., the mixture was diluted with water and adjusted to pH2. After extraction with ethyl acetate, the organic layer was washed with water and then brine, dried (MgSO4) and the solvent evaporated. The solid was filtered off, washed with hexane and dried under vacuum to give 5-benzyloxy-2-fluoro-4-methylnitrobenzene (4.83 g, 80%).