Potassium Carbonate → Methyl 2-(4-acetyl-2-bromophenoxy)acetate

HRID 68597

반응식

HRID 68597 반응식
[Br:1][C:2]1[CH:3]=[C:4]([C:9](=[O:11])[CH3:10])[CH:5]=[CH:6][C:7]=1[OH:8].Br[CH2:13][C:14]([O:16][CH3:17])=[O:15].C(=O)([O-])[O-].[K+].[K+]>CN(C=O)C>[C:9]([C:4]1[CH:5]=[CH:6][C:7]([O:8][CH2:13][C:14]([O:16][CH3:17])=[O:15])=[C:2]([Br:1])[CH:3]=1)(=[O:11])[CH3:10]

참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 60984Methyl bromoacetateHCID 6080941-(3-Bromo-4-hydroxyphenyl)ethanone

생성물 1

HCID 66868355Methyl 2-(4-acetyl-2-bromophenoxy)acetate수율 81%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

To a solution of 1-(3-bromo-4-hydroxyphenyl)ethanone (15) (963 mg, 4.48 mmol, 1 eq, Aldrich, Milwaukee, Wis., USA) in DMF (15 mL), was added methyl 2-bromoacetate (1.02 g, 6.72 mmol, 1.5 eq) and potassium carbonate (1.86 g, 13.5 mmol; 3 eq). The reaction mixture was stirred at room temperature for 18 h. Solvent was removed in vacuo, and the residue was dissolved in EtOAc, washed by water and brine, dried (Na2SO4), filtered, and concentrated in vacuo to give 1.05 g, (81%) of methyl 2-(4-acetyl-2-bromophenoxy)acetate (16) as a brown solid.

후처리

  1. customSolvent was removed in vacuo
  2. dissolutionthe residue was dissolved in EtOAc
  3. washwashed by water and brine
  4. dry with materialdried (Na2SO4)
  5. filtrationfiltered
  6. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-53bed643add440ce9aa0f42a890cfb39
출처 데이터셋
uspto-grants-2014_09
특허 번호
US08822467B2

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