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

HRID 361908ノート

反応式

HRID 361908 の反応式
[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]

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 1118Sulfuric Acid触媒

反応条件

温度
100 °C

実験手順

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.

後処理

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

出典と根拠

ORDレコード
ord-4cdbf89a82754d4d83f635c2a5599fc0
出典データセット
uspto-grants-1999_02
特許番号
US05866577

反応ノート

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