Trifluoroacetic acid → HCID 11177225, Verbindung

HRID 1172572

Reaktionsgleichung

Reaktionsgleichung von HRID 1172572
C(O)(C(F)(F)F)=O.[CH:8]12[CH2:14][CH:11]([NH:12][CH2:13]1)[CH2:10][N:9]2[C:15]1[N:20]=[C:19]([NH2:21])[N:18]2[N:22]=[C:23]([C:25]3[O:26][CH:27]=[CH:28][CH:29]=3)[N:24]=[C:17]2[CH:16]=1.Cl[CH2:31][C:32]1[C:33]([CH3:38])=[N:34][O:35][C:36]=1[CH3:37].CCN(CC)CC>CC#N>[CH3:38][C:33]1[C:32]([CH2:31][N:12]2[CH2:13][CH:8]3[CH2:14][CH:11]2[CH2:10][N:9]3[C:15]2[N:20]=[C:19]([NH2:21])[N:18]3[N:22]=[C:23]([C:25]4[O:26][CH:27]=[CH:28][CH:29]=4)[N:24]=[C:17]3[CH:16]=2)=[C:36]([CH3:37])[O:35][N:34]=1

Komponenten

6

Edukt 4

HCID 6422Trifluoroacetic acidHCID 8471TriethylamineHCID 88246Isoxazole, 4-(chloromethyl)-3,5-dimethyl-HCID 686862367-(2,5-Diaza-bicyclo[2.2.1]hept-2-yl)-2-furan-2-yl-[1,2,4]triazolo[1,5-c]pyrimidin-5-ylamine

Produkt 1

HCID 11177225HCID 11177225, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6342AcetonitrileLösungsmittel

Versuchsvorschrift

The TFA salt of 7-(2,5-diaza-bicyclo[2.2.1]hept-2-yl)-2-furan-2-yl-[1,2,4]triazolo[1,5-c]pyrimidin-5-ylamine (0.3 mmol; see Example 18 above) was dissolved in 3 mL of CH3CN along with 0.3 mmol of 4-chloromethyl-3,5-dimethyl-isoxazole (Aldrich-Sigma, St. Louis, Mo.) and 0.5 mmol of Et3N. The reaction mixture was stirred at room temperature for 18 hours. It was then concentrated and purified by preparative HPLC to afford the title compound. 1H NMR (400 Hz, DMSO-d6) δ 7.80 (d, J=1.0 Hz, 1H), 7.00 (d, J=3.6 Hz, 1H), 6.60 (dd, J=3.6, 1.0 Hz, 1H), 5.7 (s, 1H), 4.80 (brs, 2H), 2.4-3.6 (m, 14H). MS m/z: 407 [M+H]+.

Aufarbeitung

  1. concentrationIt was then concentrated
  2. custompurified by preparative HPLC

Quellen und Nachweise

ORD-Eintrag
ord-ff1540c77f164a4ebdad0305a39bbe0a
Quelldatensatz
uspto-grants-2010_11
Patentnummer
US07834014B2

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