Ethanol → Ethyl 2-(3,4-dimethoxyphenyl)-2-methylpropanoate

HRID 1627395노트

반응식

HRID 1627395 반응식
[CH3:1][O:2][C:3]1[CH:4]=[C:5]([C:11]([CH3:16])([CH3:15])[C:12]([OH:14])=[O:13])[CH:6]=[CH:7][C:8]=1[O:9][CH3:10].OS(O)(=O)=O.[CH3:22][CH2:23]O>>[CH3:1][O:2][C:3]1[CH:4]=[C:5]([C:11]([CH3:16])([CH3:15])[C:12]([O:14][CH2:22][CH3:23])=[O:13])[CH:6]=[CH:7][C:8]=1[O:9][CH3:10]

참가 물질

4

반응물 3

HCID 702EthanolHCID 1118Sulfuric AcidHCID 122597132-(3,4-Dimethoxyphenyl)-2-methylpropanoic acid

생성물 1

HCID 20523075Ethyl 2-(3,4-dimethoxyphenyl)-2-methylpropanoate

실험 절차

A solution of 2-(3,4-dimethoxyphenyl)-2-methylpropanoic acid (2.5 g, 11.15 mmol) in EtOH (50 mL) with H2SO4 (cat.) was heated at reflux 12 h. The mixture was cooled to room temperature and the solvent was evaporated under reduced pressure. The residue was dissolved in EtOAc and washed with satd NaHCO3 and brine. The organic layer was dried over MgSO4, filtered and concentrated to give ethyl 2-(3,4-dimethoxyphenyl)-2-methylpropanoate (2.81 g, quant), which was used without further purification. 1H NMR (400 MHz, CDCl3) δ 6.95-6.78 (m, 3H), 4.14 (q, 2H), 3.88 (s, 3H), 3.87 (s, 3H), 1.56 (s, 6H), 1.19 (t. 3H).

후처리

  1. temperatureat reflux 12 h
  2. customthe solvent was evaporated under reduced pressure
  3. dissolutionThe residue was dissolved in EtOAc
  4. washwashed with satd NaHCO3 and brine
  5. dry with materialThe organic layer was dried over MgSO4
  6. filtrationfiltered
  7. concentrationconcentrated

출처 및 근거

ORD 기록
ord-905bafa706184d05b3f63e0d7c5535ac
출처 데이터셋
uspto-grants-2014_07
특허 번호
US08785488B2

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