Trifluoroacetic acid → HCID 178419102, Verbindung

HRID 10466

Reaktionsgleichung

Reaktionsgleichung von HRID 10466
[C:1]1([CH:7]([C:30]2[CH:35]=[CH:34][CH:33]=[CH:32][CH:31]=2)[CH2:8][NH:9][C:10]2[N:18]=[C:17]([C:19]([O:21][CH2:22][CH3:23])=[O:20])[N:16]=[C:15]3[C:11]=2[N:12]=[CH:13][N:14]3C2CCCCO2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.FC(F)(F)C(O)=O>C(O)C>[C:30]1([CH:7]([C:1]2[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=2)[CH2:8][NH:9][C:10]2[N:18]=[C:17]([C:19]([O:21][CH2:22][CH3:23])=[O:20])[N:16]=[C:15]3[C:11]=2[N:12]=[CH:13][NH:14]3)[CH:31]=[CH:32][CH:33]=[CH:34][CH:35]=1

Komponenten

4

Edukt 2

HCID 6422Trifluoroacetic acidHCID 21978293Ethyl 6-[(2,2-diphenylethyl)amino]-9-(tetrahydro-2H-pyran-2-yl)-9H-purine-2-carboxylate

Produkt 1

HCID 178419102HCID 178419102, VerbindungAusbeute 100,6 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 702EthanolLösungsmittel

Versuchsvorschrift

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.

Aufarbeitung

  1. temperatureThe mixture was cooled
  2. filtrationthe solid was collected by filtration
  3. washThe filter cake was washed with absolute ethanol (350 ml)
  4. customwas then dried in vacuo at 50° C.

Quellen und Nachweise

ORD-Eintrag
ord-81c01a4908cd47028c7b6659b5d734b4
Quelldatensatz
uspto-grants-2006_08
Patentnummer
US07094769B2

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