Potassium Carbonate → 2,4-Dibromo-1-(methoxymethoxy)benzene

HRID 455562

반응식

HRID 455562 반응식
[Br:1][C:2]1[CH:7]=[C:6]([Br:8])[CH:5]=[CH:4][C:3]=1[OH:9].C(=O)([O-])[O-].[K+].[K+].[CH2:16]([O:18][CH2:19]Cl)C>CC(C)=O>[Br:1][C:2]1[CH:7]=[C:6]([Br:8])[CH:5]=[CH:4][C:3]=1[O:9][CH2:16][O:18][CH3:19]

참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 120052,4-DibromophenolHCID 18523Chloromethyl ethyl ether

생성물 1

HCID 105658332,4-Dibromo-1-(methoxymethoxy)benzene수율 91.6%

시약·촉매·용매 1

HCID 180Acetone용매

실험 절차

A flask was charged with 2,4-dibromophenol (50.4 g, 200 mmol), potassium carbonate (69.1 g, 500 mmol) and acetone (500 mL). The suspension was stirred at RT for 30 minutes and then treated dropwise with chloromethyl ethyl ether (19 mL, 213 mmol). After 3 h at RT the mixture was filtered and the filtrate was partitioned between EtOAc and water. The organic phase was separated, washed with water, aqueous saturated NaHCO3 and brine. The organic phase was dried over MgSO4 and the solvent was removed under reduced pressure to afford 54.2 g 2,4-dibromo-1-(methoxymethoxy)benzene, which was used in the next step without further purification.

후처리

  1. filtrationAfter 3 h at RT the mixture was filtered
  2. customthe filtrate was partitioned between EtOAc and water
  3. customThe organic phase was separated
  4. washwashed with water, aqueous saturated NaHCO3 and brine
  5. dry with materialThe organic phase was dried over MgSO4
  6. customthe solvent was removed under reduced pressure

출처 및 근거

ORD 기록
ord-4b667f142e684da0993cc7994ceaa4d4
출처 데이터셋
uspto-grants-2013_07
특허 번호
US08497264B2

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