3-Amino-1-propanol → 9-Ethyl-2-(3-hydroxy-propyl-amino)-6-(3-trifluoromethyl-phenyl-amino)-9H-purine

HRID 9900

反応式

HRID 9900 の反応式
Cl[C:2]1[N:10]=[C:9]2[C:5]([N:6]=[CH:7][N:8]2[CH2:11][CH3:12])=[C:4]([NH:13][C:14]2[CH:19]=[CH:18][CH:17]=[C:16]([C:20]([F:23])([F:22])[F:21])[CH:15]=2)[N:3]=1.[NH2:24][CH2:25][CH2:26][CH2:27][OH:28]>C(OCC)(=O)C>[CH2:11]([N:8]1[CH:7]=[N:6][C:5]2[C:9]1=[N:10][C:2]([NH:24][CH2:25][CH2:26][CH2:27][OH:28])=[N:3][C:4]=2[NH:13][C:14]1[CH:19]=[CH:18][CH:17]=[C:16]([C:20]([F:23])([F:22])[F:21])[CH:15]=1)[CH3:12]

参加物

4

反応物 2

HCID 90863-Amino-1-propanolHCID 219881872-chloro-9-ethyl-6-(3-trifluoromethyl-phenyl-amino)-9H-purine

生成物 1

HCID 219882069-Ethyl-2-(3-hydroxy-propyl-amino)-6-(3-trifluoromethyl-phenyl-amino)-9H-purine

試薬・触媒・溶媒 1

HCID 8857Ethyl Acetate溶媒

実験手順

200 mg (0.58 mmol) of 2-chloro-9-ethyl-6-(3-trifluoromethyl-phenyl-amino)-9H-purine and 2 ml of 3-amino-1-propanol are stirred at 140° C. for 2 h and the mixture is allowed to cool and is diluted with 60 ml of ethyl acetate. The organic phase is washed with water and dried over sodium sulfate. After removal of the solvent, the residue is recrystallized from ethyl acetate and diethyl ether. 9-Ethyl-2-(3-hydroxy-propyl-amino)-6-(3-trifluoromethyl-phenyl-amino)-9H-purine is obtained; m.p. 136–137° C.; FAB-MS: (M+H)+=381; Rf=0.7 (ethyl acetate:methanol=9:1).

後処理

  1. temperatureto cool
  2. washThe organic phase is washed with water
  3. dry with materialdried over sodium sulfate
  4. customAfter removal of the solvent
  5. customthe residue is recrystallized from ethyl acetate and diethyl ether

出典と根拠

ORDレコード
ord-3a5c495ce8bd459ab04cfd5ab755e0c5
出典データセット
uspto-grants-2006_08
特許番号
US07091346B1

関連ノート

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