Methyl iodide → HCID 22996212、化合物

HRID 1167295

反応式

HRID 1167295 の反応式
[Br:1][C:2]1[CH:7]=[CH:6][C:5]([OH:8])=[CH:4][C:3]=1[O:9][CH2:10][CH2:11][CH3:12].[C:13](=O)([O-])[O-].[K+].[K+].CI>CC(C)=O>[Br:1][C:2]1[CH:7]=[CH:6][C:5]([O:8][CH3:13])=[CH:4][C:3]=1[O:9][CH2:10][CH2:11][CH3:12]

参加物

5

反応物 3

HCID 6328Methyl iodideHCID 11430Potassium CarbonateHCID 229961784-Bromo-3-propoxy-phenol

生成物 1

HCID 22996212HCID 22996212、化合物収率 97.1%

試薬・触媒・溶媒 1

HCID 180Acetone溶媒

実験手順

To a solution of 4-bromo-3-propoxy-phenol (500 mg, 2.164 mmol) in acetone (10 mL) were added potassium carbonate (299 mg, 2.164 mmol) and methyl iodide (674 μL, 10.82 mmol). The reaction mixture was heated at gentle reflux for 12 h. The solvent was removed and the residue was taken in diethyl ether (50 mL). The white solid was filtered off, and the filtrated was concentrated in vacuo. Purification of the crude residue by flash chromatography (Biotage system, KP-Sil™ 32-63 μm, 60 Å silica gel) eluting with 5-10% ethyl acetate in hexanes yielded 1-bromo-4-methoxy-2-propoxy-benzene as a clear oil (515 mg, 97%).

後処理

  1. temperatureThe reaction mixture was heated
  2. temperatureat gentle reflux for 12 h
  3. customThe solvent was removed
  4. filtrationThe white solid was filtered off
  5. concentrationthe filtrated was concentrated in vacuo
  6. customPurification of the crude residue by flash chromatography (Biotage system, KP-Sil™ 32-63 μm, 60 Å silica gel)
  7. washeluting with 5-10% ethyl acetate in hexanes

出典と根拠

ORDレコード
ord-6a9d5e8751a747bb99f4fd51da30ab0c
出典データセット
uspto-grants-2003_09
特許番号
US06617346B1

関連ノート

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