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

HRID 361908笔记

反应方程式

HRID 361908 反应方程式
[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]

参与物

5

反应物 3

HCID 702乙醇HCID 755826-甲氧基-3,4-二氢-1H-2-萘酮HCID 53630039Ethylorthoformate

产物 1

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

试剂、催化剂与溶剂 1

HCID 1118四氧化硫催化剂

反应条件

温度
100 °C

实验过程

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.

后处理

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

来源与证据

ORD记录
ord-4cdbf89a82754d4d83f635c2a5599fc0
来源数据集
uspto-grants-1999_02
专利号
US05866577

反应笔记

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