반응 #595333

ord-5970614c3a9c4a1f96ec574ef8d59127

반응 방정식

O=Cc1ccc(O)c(F)c1
3-fluoro-4-hydroxybenzaldehyde
OCCBr
2-bromoethanol
O=C([O-])[O-].[K+].[K+]
potassium carbonate
O=Cc1ccc(OCCO)c(F)c1
3-Fluoro-4-(2-hydroxyethoxy)benzaldehyde

용매

반응 조건

온도
150°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    여과The mixture is then filtered
  2. 2
    기타the filtrate is freed from the solvent on a rotary evaporator
  3. 3
    workup.ADDITION20 ml of sat. aqueous sodium bicarbonate solution are added
  4. 4
    기타The phases are separated
  5. 5
    건조the organic phase is dried over magnesium sulfate
  6. 6
    기타The solvent is removed on a rotary evaporator
  7. 7
    기타The product obtained
  8. 8
    기타is used without further purification in the subsequent reaction

실험 절차

5.00 g (35.69 mmol) of 3-fluoro-4-hydroxybenzaldehyde are dissolved in 50 ml of dry DMF. 5.35 g (42.82 mmol) of 2-bromoethanol and 19.73 g (142.74 mmol) of potassium carbonate are added. The reaction mixture is stirred at 150° C. for 10 h. The mixture is then filtered, and the filtrate is freed from the solvent on a rotary evaporator. The residue is taken up in 30 ml of ethyl acetate, and 20 ml of sat. aqueous sodium bicarbonate solution are added. The phases are separated and the organic phase is dried over magnesium sulfate. The solvent is removed on a rotary evaporator. The product obtained is used without further purification in the subsequent reaction.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US09095582B2uspto-grants-2015_08