반응 #43928

반응 방정식

Ethyl acetate

4-bromo-3-(bromomethyl)-5-methylphenyl acetate

sodium acetate

→

title compound

수율 67.0%

5-acetoxy-2-bromo-3-methylbenzyl acetate

수율 67.0%

용매

N,N-dimethylformamide

반응 조건

후처리

1. 1
   세척the mixture was washed successively with water and saturated brine
2. 2
   건조dried over anhydrous magnesium sulfate
3. 3
   농축concentrated under reduced pressure
4. 4
   기타The residue was purified by silica gel column chromatography (ethyl acetate:hexane=0:100-25:75)

실험 절차

To a solution of 4-bromo-3-(bromomethyl)-5-methylphenyl acetate (11.7 g, 36.3 mmol) in N,N-dimethylformamide (60 mL) was added sodium acetate (5.96 g, 72.6 mmol), and the mixture was stirred at 70° C. for 4 hr under nitrogen atmosphere. Ethyl acetate was added to the reaction mixture, and the mixture was washed successively with water and saturated brine, dried over anhydrous magnesium sulfate, and concentrated under reduced pressure. The residue was purified by silica gel column chromatography (ethyl acetate:hexane=0:100-25:75) to give the title compound (7.29 g, yield 67%) as a pale-yellow oil.

출처