반응 #2146691

반응 방정식

4′-benzoyloxyacetophenone

tetra-n-butyl ammonium tribromide

→

4′-benzoyloxy-2-bromoacetophenone

수율 73.5%

용매

methanol

반응 조건

후처리

1. 1
   workup.DISTILLATIONwas distilled off under reduced pressure
2. 2
   기타to remove the solvent
3. 3
   workup.DISSOLUTIONThe residue was dissolved in ethyl acetate
4. 4
   세척washed twice with water
5. 5
   세척washed with an aqueous saturated sodium chloride solution
6. 6
   건조After the ethyl acetate layer was dried over anhydrous sodium sulfate
7. 7
   농축concentrated under reduced pressure
8. 8
   기타the resulting crude product was purified by silica gel column chromatography (elution solvent: hexane/methylene chloride=1/1)

실험 절차

13.50 g (corresponding to 59.66 mmol) of 4′-benzoyloxyacetophenone was dissolved in 1100 ml of methanol, and 34.52 g (corresponding to 71.59 mmol) of tetra-n-butyl ammonium tribromide was added thereto. The mixture was stirred overnight at room temperature, and was distilled off under reduced pressure to remove the solvent. The residue was dissolved in ethyl acetate and washed twice with water and then washed with an aqueous saturated sodium chloride solution. After the ethyl acetate layer was dried over anhydrous sodium sulfate and concentrated under reduced pressure, the resulting crude product was purified by silica gel column chromatography (elution solvent: hexane/methylene chloride=1/1), to obtain 13.38 g (corresponding to 43.84 mmol) of 4′-benzoyloxy-2-bromoacetophenone (FIG. 3, Step 4).

출처