Water → 3-Bromo-4-ethoxybenzonitrile

HRID 1865040

反応式

HRID 1865040 の反応式
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]

参加物

6

反応物 4

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

生成物 1

HCID 22390723-Bromo-4-ethoxybenzonitrile

試薬・触媒・溶媒 1

HCID 180Acetone溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-52df170b0f6f49aab8a21edd1c1df123
出典データセット
uspto-grants-2009_12
特許番号
US07625932B2

関連ノート

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