반응 #9996

ord-3a5c495ce8bd459ab04cfd5ab755e0c5

반응 방정식

CCn1cnc2c(Nc3cccc(C(F)(F)F)c3)nc(Cl)nc21
2-chloro-9-ethyl-6-(3-trifluoromethyl-phenyl-amino)-9H-purine
NCCCO
3-amino-1-propanol
CCn1cnc2c(Nc3cccc(C(F)(F)F)c3)nc(NCCCO)nc21
9-Ethyl-2-(3-hydroxy-propyl-amino)-6-(3-trifluoromethyl-phenyl-amino)-9H-purine

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도to cool
  2. 2
    세척The organic phase is washed with water
  3. 3
    건조dried over sodium sulfate
  4. 4
    기타After removal of the solvent
  5. 5
    기타the residue is recrystallized from ethyl acetate and diethyl ether

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).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US07091346B1uspto-grants-2006_08