Sodium Methoxide → 5-Bromo-2-(7-methoxyheptyloxy)-1,3-dimethylbenzene

HRID 1816726

反応式

HRID 1816726 の反応式
[Br:1][C:2]1[CH:3]=[C:4]([CH3:18])[C:5]([O:9][CH2:10][CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][CH2:16]Br)=[C:6]([CH3:8])[CH:7]=1.[CH3:19][O-:20].[Na+]>CO>[Br:1][C:2]1[CH:3]=[C:4]([CH3:18])[C:5]([O:9][CH2:10][CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][CH2:16][O:20][CH3:19])=[C:6]([CH3:8])[CH:7]=1

参加物

4

反応物 2

HCID 10942334Sodium MethoxideHCID 224946365-Bromo-2-(7-bromoheptyloxy)-1,3-dimethylbenzene

生成物 1

HCID 224947715-Bromo-2-(7-methoxyheptyloxy)-1,3-dimethylbenzene

試薬・触媒・溶媒 1

HCID 887Methanol溶媒2 回

実験手順

A solution of crude 5-bromo-2-(7-bromoheptyloxy)-1,3-dimethylbenzene (7.81 g) in methanol (78 ml) was treated with 28% sodium methoxide in methanol (78 ml), and the solution was refluxed for 8 hours. After cooling, the reaction mixture was evaporated under reduced pressure, and the residue was extracted with methylene chloride. The organic layer was dried over magnesium sulfate and magnesium sulfate was filtered off, and then the filtrate was evaporated under reduced pressure. The residue was purified by silica gel column chromatography eluting with a mixed solvent of n-hexane-ethyl acetate (from 0% to 7% gradient elution) to give 5-bromo-2-(7-methoxyheptyloxy)-1,3-dimethylbenzene (3.34 g) as a colorless oil.

後処理

  1. temperaturethe solution was refluxed for 8 hours
  2. temperatureAfter cooling
  3. customthe reaction mixture was evaporated under reduced pressure
  4. extractionthe residue was extracted with methylene chloride
  5. dry with materialThe organic layer was dried over magnesium sulfate and magnesium sulfate
  6. filtrationwas filtered off
  7. customthe filtrate was evaporated under reduced pressure
  8. customThe residue was purified by silica gel column chromatography
  9. washeluting with a mixed solvent of n-hexane-ethyl acetate (from 0% to 7% gradient elution)

出典と根拠

ORDレコード
ord-f2cfa733b5be49458a48c3a789d932ac
出典データセット
uspto-grants-2005_04
特許番号
US06884868B1

関連ノート

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