تفاعل #9996

ord-3a5c495ce8bd459ab04cfd5ab755e0c5

معادلة التفاعل

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

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    درجة الحرارةto cool
  2. 2
    غسيلThe organic phase is washed with water
  3. 3
    تجفيفdried over sodium sulfate
  4. 4
    أخرىAfter removal of the solvent
  5. 5
    أخرىthe residue is recrystallized from ethyl acetate and diethyl ether

الإجراء التجريبي

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).

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US07091346B1uspto-grants-2006_08