Ethanol → 3-Ethoxy-7-methoxy-1,2-dihydronaphthalene

HRID 1738686

반응식

HRID 1738686 반응식
[CH3:1][O:2][C:3]1[CH:4]=[C:5]2[C:10](=[CH:11][CH:12]=1)[CH2:9][C:8](=O)[CH2:7][CH2:6]2.C([O-])([O-])OCC.[CH2:20]([OH:22])[CH3:21]>S(=O)(=O)(O)O>[CH2:20]([O:22][C:8]1[CH2:7][CH2:6][C:5]2[C:10](=[CH:11][CH:12]=[C:3]([O:2][CH3:1])[CH:4]=2)[CH:9]=1)[CH3:21]

참가 물질

5

반응물 3

HCID 702EthanolHCID 755826-Methoxy-1,2,3,4-tetrahydronaphthalen-2-oneHCID 53630039Ethylorthoformate

생성물 1

HCID 218442353-Ethoxy-7-methoxy-1,2-dihydronaphthalene

시약·촉매·용매 1

HCID 1118Sulfuric Acid촉매

반응 조건

온도
100 °C

실험 절차

33.5 g of 6-methoxy-2-tetralone was dissolved in 27.6 ml of ethanol, followed by subsequently adding 37.8 ml of ethyl orthoformate and one drop of concentrated sulfuric acid. The mixture thus prepared was stirred at 100° C. for 4 hours. After distilling off the solvent under a reduced pressure, the resulting residue was subjected to silica gel column chromatography using chloroform as an eluant. Fractions of interest were pooled and concentrated to collect precipitated crystals, thereby obtaining 5.82 g of 3,4-dihydro-2-ethoxy-6-methoxynaphthalene.

후처리

  1. customThe mixture thus prepared
  2. distillationAfter distilling off the solvent under a reduced pressure
  3. concentrationconcentrated
  4. customto collect
  5. customprecipitated crystals

출처 및 근거

ORD 기록
ord-57d593158a8a49518757bb74bd1ff41a
출처 데이터셋
uspto-grants-1999_10
특허 번호
US05962695

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