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

HRID 2305

反応式

HRID 2305 の反応式
Cl[C:2]1[N:7]=[CH:6][N:5]=[C:4]([NH2:8])[C:3]=1[C:9]1[CH:14]=[CH:13][C:12]([CH3:15])=[CH:11][CH:10]=1.[H-].[Na+].[Cl-].[NH4+].[CH2:20]([OH:23])[CH2:21][OH:22]>>[NH2:8][C:4]1[N:5]=[CH:6][N:7]=[C:2]([O:22][CH2:21][CH2:20][OH:23])[C:3]=1[C:9]1[CH:14]=[CH:13][C:12]([CH3:15])=[CH:11][CH:10]=1

参加物

5

反応物 4

HCID 174Ethylene GlycolHCID 24758Sodium hydrideHCID 25517Ammonium ChlorideHCID 189311004-Amino-6-chloro-5-(4-methylphenyl)pyrimidine

生成物 1

HCID 111182972-{6-Amino-5-(4-methylphenyl)-pyrimidin-4-yloxy}ethanol

実験手順

A mixture of 6-chloro-5-(4-methylphenyl)pyrimidin-4-amine (500 mg), ethylene glycol (10 ml) and sodium hydride (60% dispersion-type, 0.46 g) is reacted at 70° C. for two hours, and reacted at 90° C. for five hours. The mixture is treated with saturated aqueous ammonium chloride solution, and extracted with ethyl acetate. The ethyl acetate layer is washed, dried, and evaporated to remove the solvent. The residue is crystallized from hexane/ethyl acetate to give 2-{6-amino-5-(4-methylphenyl)pyrimidin-4-yloxy}-ethanol (422 mg).

後処理

  1. customis reacted at 70° C. for two hours
  2. customreacted at 90° C. for five hours
  3. extractionextracted with ethyl acetate
  4. washThe ethyl acetate layer is washed
  5. customdried
  6. customevaporated
  7. customto remove the solvent
  8. customThe residue is crystallized from hexane/ethyl acetate

出典と根拠

ORDレコード
ord-c45d1e41cd734870bba0fc8cf09b8c4c
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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