反応 #2407

ord-f570953042144533ac7122491f64e455

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    温度cooling
  2. 2
    その他evaporated
  3. 3
    その他to remove the solvent
  4. 4
    抽出The residue is extracted with ethyl acetate
  5. 5
    抽出the ethyl acetate extract
  6. 6
    その他is dried
  7. 7
    濃縮concentrated under reduced pressure
  8. 8
    その他The residue is purified by silica gel column chromatography (solvent; chloroform/ethyl acetate=5:1~2:1)

実験手順

To a mixture of 4,6-dichloropyrimidine (5.0 g), ethylene glycol (100 ml) and tetrahydrofuran (100 ml)is added sodium hydride (60% dispersion-type, 1.34 g) under ice-cooling. The mixture is stirred at the same temperature for two hours, and evaporated to remove the solvent. The residue is extracted with ethyl acetate, and the ethyl acetate extract is dried, and concentrated under reduced pressure. The residue is purified by silica gel column chromatography (solvent; chloroform/ethyl acetate=5:1~2:1) to give 2-(6-chloropyrimidin-4-yloxy)ethanol (5.67 g) as an oily product.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US05728706uspto-grants-1998_03