Water → 3-Bromo-4-ethoxybenzonitrile

HRID 1865040

반응식

HRID 1865040 반응식
C(=O)([O-])[O-].[K+].[K+].[Br:7][C:8]1[CH:9]=[C:10]([CH:13]=[CH:14][C:15]=1[OH:16])[C:11]#[N:12].I[CH2:18][CH3:19].O>CC(C)=O>[Br:7][C:8]1[CH:9]=[C:10]([CH:13]=[CH:14][C:15]=1[O:16][CH2:18][CH3:19])[C:11]#[N:12]

참가 물질

6

반응물 4

HCID 962WaterHCID 6340IodoethaneHCID 11430Potassium CarbonateHCID 753413-Bromo-4-hydroxybenzonitrile

생성물 1

HCID 22390723-Bromo-4-ethoxybenzonitrile

시약·촉매·용매 1

HCID 180Acetone용매

실험 절차

Add potassium carbonate (5.2 g, 37.9 mmol) to 3-bromo-4-hydroxy-benzonitrile (5.0 g, 25.2 mmol) in acetone with stirring at room temperature. After 15 minutes, add iodoethane (2.4 mL, 130.3 mmol) and continue stirring at room temperature. After 18 hours, pour the reaction mixture into water and extract with EtOAc. Combine the organic extracts, wash with water and brine, dry over anhydrous magnesium sulfate, filter, and concentrate under reduced pressure. Purify the residue by flash chromatography eluting with ethyl acetate:hexanes to provide the title compound.

후처리

  1. stirringcontinue stirring at room temperature
  2. waitAfter 18 hours
  3. extractionextract with EtOAc
  4. washwash with water and brine
  5. dry with materialdry over anhydrous magnesium sulfate
  6. filtrationfilter
  7. concentrationconcentrate under reduced pressure
  8. customPurify the residue by flash chromatography
  9. washeluting with ethyl acetate

출처 및 근거

ORD 기록
ord-52df170b0f6f49aab8a21edd1c1df123
출처 데이터셋
uspto-grants-2009_12
특허 번호
US07625932B2

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