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

HRID 1816726

반응식

HRID 1816726 반응식
[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

참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 887Methanol용매2회

실험 절차

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.

후처리

  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)

출처 및 근거

ORD 기록
ord-f2cfa733b5be49458a48c3a789d932ac
출처 데이터셋
uspto-grants-2005_04
특허 번호
US06884868B1

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