تفاعل #43942

معادلة التفاعل

2-fluoro-4-hydroxybenzaldehyde

bromine

→

title compound

المردود 81.2%

5-bromo-2-fluoro-4-hydroxybenzaldehyde

المردود 81.2%

المذيبات

acetic acid

acetic acid

ظروف التفاعل

المعالجة

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

الإجراء التجريبي

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.

المصدر