Ethylene Glycol → 2-[(6-Chloropyrimidin-4-yl)oxy]ethan-1-ol

HRID 2311

反応式

HRID 2311 の反応式
[Cl:1][C:2]1[CH:7]=[C:6](Cl)[N:5]=[CH:4][N:3]=1.[CH2:9]([OH:12])[CH2:10][OH:11].[H-].[Na+]>O1CCCC1>[Cl:1][C:2]1[N:3]=[CH:4][N:5]=[C:6]([O:11][CH2:10][CH2:9][OH:12])[CH:7]=1

参加物

5

反応物 3

HCID 174Ethylene GlycolHCID 24758Sodium hydrideHCID 709434,6-Dichloropyrimidine

生成物 1

HCID 125648862-[(6-Chloropyrimidin-4-yl)oxy]ethan-1-ol

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

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.

後処理

  1. temperaturecooling
  2. customevaporated
  3. customto remove the solvent
  4. extractionThe residue is extracted with ethyl acetate
  5. extractionthe ethyl acetate extract
  6. customis dried
  7. concentrationconcentrated under reduced pressure
  8. customThe residue is purified by silica gel column chromatography (solvent; chloroform/ethyl acetate=5:1~2:1)

出典と根拠

ORDレコード
ord-f570953042144533ac7122491f64e455
出典データセット
uspto-grants-1998_03
特許番号
US05728706

関連ノート

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