Propargyl bromide → 5-Bromo-1,2-difluoro-3-prop-2-ynyloxybenzene

HRID 2244844노트

반응식

HRID 2244844 반응식
[Br:1][C:2]1[CH:3]=[C:4]([F:10])[C:5]([F:9])=[C:6]([OH:8])[CH:7]=1.[CH2:11](Br)[C:12]#[CH:13].C(=O)([O-])[O-].[K+].[K+]>CC(CC)=O>[Br:1][C:2]1[CH:7]=[C:6]([O:8][CH2:13][C:12]#[CH:11])[C:5]([F:9])=[C:4]([F:10])[CH:3]=1

참가 물질

5

반응물 3

HCID 7842Propargyl bromideHCID 11430Potassium CarbonateHCID 27733075-Bromo-2,3-Difluorophenol

생성물 1

HCID 592152525-Bromo-1,2-difluoro-3-prop-2-ynyloxybenzene

시약·촉매·용매 1

HCID 6569Methyl Ethyl Ketone용매

실험 절차

50.0 g (0.24 mol) of 5-bromo-2,3-difluorophenol are refluxed for 3 h together with 32.0 ml (0.29 mol) of propargyl bromide (80% soln. in toluene) and 39.7 g (0.29 mol) of potassium carbonate in 860 ml of ethyl methyl ketone. The batch is filtered, and the filter residue is washed with MTBE. The filtrate is concentrated to dryness, and the residue is purified by column chromatography (SiO2, n-heptane:MTBE=3:1).

후처리

  1. filtrationThe batch is filtered
  2. washthe filter residue is washed with MTBE
  3. concentrationThe filtrate is concentrated to dryness
  4. customthe residue is purified by column chromatography (SiO2, n-heptane:MTBE=3:1)

출처 및 근거

ORD 기록
ord-bb35b0ddd6654b0c9dc938195de1d6ce
출처 데이터셋
uspto-grants-2010_03
특허 번호
US07678929B2

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