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

HRID 1599029

반응식

HRID 1599029 반응식
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

참가 물질

6

반응물 4

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

생성물 1

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

시약·촉매·용매 1

HCID 176Acetic Acid용매

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-443b6a410d644885b063dcd42d3ef063
출처 데이터셋
uspto-grants-1998_04
특허 번호
US05739333

연결된 노트

불러오는 중…