1,4-Dioxane → HCID 19014324, Verbindung

HRID 1728549Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1728549
[CH3:1][C:2]1[N:3]=[C:4]([NH:17][CH3:18])[C:5]2[CH:10]=[CH:9][N:8]([C:11]3[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=3)[C:6]=2[N:7]=1.O1CCOC[CH2:20]1>>[CH3:1][C:2]1[N:3]([CH3:20])[C:4](=[N:17][CH3:18])[C:5]2[CH:10]=[CH:9][N:8]([C:11]3[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=3)[C:6]=2[N:7]=1

Komponenten

3

Edukt 2

HCID 312751,4-DioxaneHCID 19014333N,2-Dimethyl-7-phenyl-7H-pyrrolo[2,3-d]pyrimidin-4-amine

Produkt 1

HCID 19014324HCID 19014324, Verbindung

Versuchsvorschrift

A mixture of 2-methyl-4-methylamino-7-phenyl-7H-pyrrolo-[2,3-d] pyrimidine (0.5g, 2.1mM) and dioxan (15ml) was heated under reflux for 18 hours. The mixture was cooled and then the solvent was removed by evaporation. The residue was purified by flash chromatography on ICN neutral alumina (32-63) using methylene chloride which contained an increasing amount of methanol (up to a maximum of 5%) as eluant to give a solid. This solid was recrystallised from hexane to give 2,3-dimethyl-4-methylimino-7-phenyl-3H,7H-pyrrolo[2,3-d] pyrimidine as a white solid (126mg), m p. 160-161° C; microanalysis, found: C, 71 2; H,5 9; N,22.0%; C14H14N4 requires C,71.4; H, 6.3; N, 22.2%; NMR: 2.48(3H,s,C-CH3), 3.48 (3H,s,N-CH3), 3.56(3H,s,N-CH3), 6.90(1H,d,CH), 6.97(1H,d,CH), 7.34(1H, complex, aromatic), 7.47(2H, complex, aromatic), 7.60(1H, complex, aromatic).

Aufarbeitung

  1. temperaturewas heated
  2. temperatureunder reflux for 18 hours
  3. temperatureThe mixture was cooled
  4. customthe solvent was removed by evaporation
  5. customThe residue was purified by flash chromatography on ICN neutral alumina (32-63)
  6. customto give a solid
  7. customThis solid was recrystallised from hexane

Quellen und Nachweise

ORD-Eintrag
ord-9b22da2a913e436a8f35130a03a09de6
Quelldatensatz
uspto-grants-1994_07
Patentnummer
US05328910

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