Diisopropylethylamine → HCID 86755657, Verbindung

HRID 1871992Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1871992
[CH3:1][NH:2][CH2:3][C:4]([NH:6][C:7]1[S:8][CH:9]=[C:10]([CH2:12][C:13]([O:15][CH2:16][CH3:17])=[O:14])[N:11]=1)=[O:5].C(N(CC)C(C)C)(C)C.F[C:28]1[N:33]=[C:32]([F:34])[CH:31]=[CH:30][N:29]=1>ClCCl>[F:34][C:32]1[CH:31]=[CH:30][N:29]=[C:28]([N:2]([CH3:1])[CH2:3][C:4]([NH:6][C:7]2[S:8][CH:9]=[C:10]([CH2:12][C:13]([O:15][CH2:16][CH3:17])=[O:14])[N:11]=2)=[O:5])[N:33]=1

Komponenten

5

Edukt 3

HCID 81531DiisopropylethylamineHCID 1377162,4-DifluoropyrimidineHCID 86755656HCID 86755656, Verbindung

Produkt 1

HCID 86755657HCID 86755657, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344DichloromethaneLösungsmittel

Versuchsvorschrift

The product of step (i) (3.0 g) was slurried in dichloromethane (100 ml) and treated with N,N-diisopropylethylamine (4.0 ml) forming a complete solution. 2,4-Difluoropyrimidine (J. Heterocyclic Chem. 1985, 22, 149) (0.6 g) was then added quickly with stirring. After 10 minutes the solvents were evaporated under reduced pressure and the residue purified by chromatography eluting with 20% ethyl acetate in isohexane. The first and minor component of the mixture to be eluted was the subtitle compound (0.77 g).

Aufarbeitung

  1. customforming a complete solution
  2. customAfter 10 minutes the solvents were evaporated under reduced pressure
  3. customthe residue purified by chromatography
  4. washeluting with 20% ethyl acetate in isohexane
  5. washThe first and minor component of the mixture to be eluted

Quellen und Nachweise

ORD-Eintrag
ord-6fd795cb0a5e4022bb639d3e3545ef5a
Quelldatensatz
uspto-grants-2000_08
Patentnummer
US06107297

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