Ethylene Glycol → 2-{6-Chloro-5-(4-methylphenyl)pyrimidin-4-yloxy}ethanol

HRID 1599029

反応式

HRID 1599029 の反応式
O1CCCC1.[CH2:6]([OH:9])[CH2:7][OH:8].[H-].[Na+].[Cl:12][C:13]1[C:18]([C:19]2[CH:24]=[CH:23][C:22]([CH3:25])=[CH:21][CH:20]=2)=[C:17](Cl)[N:16]=[CH:15][N:14]=1>C(O)(=O)C>[Cl:12][C:13]1[N:14]=[CH:15][N:16]=[C:17]([O:8][CH2:7][CH2:6][OH:9])[C:18]=1[C:19]1[CH:24]=[CH:23][C:22]([CH3:25])=[CH:21][CH:20]=1

参加物

6

反応物 4

HCID 174Ethylene GlycolHCID 8028TetrahydrofuranHCID 24758Sodium hydrideHCID 219795544,6-Dichloro-5-(4-methylphenyl)pyrimidine

生成物 1

HCID 111189672-{6-Chloro-5-(4-methylphenyl)pyrimidin-4-yloxy}ethanol

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

実験手順

To a mixture of tetrahydrofuran (400 ml) and ethylene glycol (60 ml) is added with stirring sodium hydride (60% dispersion, 3.38 g) under ice-cooling, and thereto is added 4,6-dichloro-5-(4-methylphenyl)pyrimidine (20.0 g). The mixture is stirred under ice-cooling for 30 minutes, and then stirred at room temperature for two hours. The mixture is weakly acidified with acetic acid, and concentrated under reduced pressure. The residue is dissolved in ethyl acetate, and washed, dried, and concentrated to dryness under reduced pressure. The residue is crystallized from hexane to give 2-{6-chloro-5-(4-methylphenyl)pyrimidin-4-yloxy}ethanol (21.85 g).

後処理

  1. temperaturecooling
  2. temperaturecooling for 30 minutes
  3. stirringstirred at room temperature for two hours
  4. concentrationconcentrated under reduced pressure
  5. dissolutionThe residue is dissolved in ethyl acetate
  6. washwashed
  7. customdried
  8. concentrationconcentrated to dryness under reduced pressure
  9. customThe residue is crystallized from hexane

出典と根拠

ORDレコード
ord-443b6a410d644885b063dcd42d3ef063
出典データセット
uspto-grants-1998_04
特許番号
US05739333

関連ノート

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