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

HRID 9900

반응식

HRID 9900 반응식
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]

참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-3a5c495ce8bd459ab04cfd5ab755e0c5
출처 데이터셋
uspto-grants-2006_08
특허 번호
US07091346B1

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