反応 #43942

反応方程式

2-fluoro-4-hydroxybenzaldehyde

bromine

→

title compound

収率 81.2%

5-bromo-2-fluoro-4-hydroxybenzaldehyde

収率 81.2%

溶媒

acetic acid

acetic acid

反応条件

後処理

1. 1
   濃縮The reaction mixture was concentrated under reduced pressure, brine
2. 2
   workup.ADDITIONwas added to the residue
3. 3
   抽出the mixture was extracted with ethyl acetate
4. 4
   乾燥The extract was dried over anhydrous magnesium sulfate
5. 5
   濃縮concentrated under reduced pressure
6. 6
   その他The residue was purified by silica gel column chromatography (ethyl acetate:hexane=5:95-40:60)

実験手順

To a solution of 2-fluoro-4-hydroxybenzaldehyde (2.16 g, 15.4 mmol) in acetic acid (70 mL) was added a solution of bromine (2.71 g, 17.0 mmol) in acetic acid (10 mL), and the mixture was stirred at 45° C. for 26 hr. The reaction mixture was concentrated under reduced pressure, brine was added to the residue, and the mixture was extracted with ethyl acetate. The extract was dried over anhydrous magnesium sulfate, and concentrated under reduced pressure. The residue was purified by silica gel column chromatography (ethyl acetate:hexane=5:95-40:60) to give the title compound (2.74 g, yield 81%) as colorless crystals.

出典