반응 #10562

ord-81c01a4908cd47028c7b6659b5d734b4

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도The mixture was cooled
  2. 2
    여과the solid was collected by filtration
  3. 3
    세척The filter cake was washed with absolute ethanol (350 ml)
  4. 4
    기타was then dried in vacuo at 50° C.

실험 절차

To a suspension of ethyl 6-[(2,2-diphenylethyl)amino]-9-(tetrahydro-2H-pyran-2-yl)-9H-purine-2-carboxylate (Preparation 62) (250 g, 0.530 moles) in absolute ethanol (1250 ml) under an atmosphere of nitrogen was added trifluoroacetic acid (73.5 g, 0.645 moles) and the resultant mixture was heated at 50° C. for 20 hours. The mixture was cooled and the solid was collected by filtration. The filter cake was washed with absolute ethanol (350 ml) and was then dried in vacuo at 50° C. to give the title compound (206.5 g) as a cream coloured fine powder, m.p. >200° C.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US07094769B2uspto-grants-2006_08