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Trifluoroacetic acid → HCID 71014653, Verbindung

HRID 2368465
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 2368465
ClC[O:3][P:4](=[O:15])([O:10][C:11](C)(C)C)[O:5]C(C)(C)C.C([O-])([O-])=O.[Cs+].[Cs+].[NH:22]1[C:30]2[C:25](=[CH:26][CH:27]=[CH:28][CH:29]=2)[C:24]([C:31]2[C:32](=[O:54])[NH:33][C:34](=[O:53])[C:35]=2[C:36]2[C:45]3[C:40](=[CH:41][CH:42]=[CH:43][CH:44]=3)[N:39]=[C:38]([N:46]3[CH2:51][CH2:50][N:49]([CH3:52])[CH2:48][CH2:47]3)[N:37]=2)=[CH:23]1.C(O)(C(F)(F)F)=O>CC(C)=O.ClCCCl.C(#N)C.CO>[NH:22]1[C:30]2[C:25](=[CH:26][CH:27]=[CH:28][CH:29]=2)[C:24]([C:31]2[C:32](=[O:54])[N:33]([CH2:11][O:10][P:4](=[O:15])([OH:3])[OH:5])[C:34](=[O:53])[C:35]=2[C:36]2[C:45]3[C:40](=[CH:41][CH:42]=[CH:43][CH:44]=3)[N:39]=[C:38]([N:46]3[CH2:51][CH2:50][N:49]([CH3:52])[CH2:48][CH2:47]3)[N:37]=2)=[CH:23]1
KomponentenReaktionsbedingungenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

9

Edukt 4

HCID 6422Trifluoroacetic acidHCID 10796Cesium carbonateHCID 102968835-Hydroxy-4-(1H-indol-3-yl)-3-[2-(4-methylpiperazin-1-yl)quinazolin-4-yl]-2H-pyrrol-2-oneHCID 11701630Di-tert-butyl (chloromethyl) phosphate

Produkt 1

HCID 71014653HCID 71014653, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 4

HCID 111,2-DichloroethaneLösungsmittel2×
HCID 180AcetoneLösungsmittel
HCID 887MethanolLösungsmittel
HCID 6342AcetonitrileLösungsmittel

Reaktionsbedingungen

Temperatur
50 °C

Versuchsvorschrift

Under argon, phosphoric acid di-tert-butyl ester chloromethyl ester (1.24 g, 4.81 mmol) and Cs2CO3 (3.14 g, 9.63 mmol) were added to a solution of 3-(1H-indol-3-yl)-4-[2-(4-methyl-piperazin-1-yl)-quinazolin-4-yl]-pyrrole-2,5-dione (2.0 g, 4.01 mmol) in acetone (40 mL). The reaction mixture was stirred under argon for 16 h at 50° C. followed by concentration at reduced pressure. The residue was partitioned between EtOAc and a saturated aqueous NH4Cl solution, the layers were separated and the organic layer was dried over anhydrous Na2SO4. Concentration at reduced pressure afforded the crude product as a red foam. The crude product was purified by reverse phase Gilson HPLC as described above. After concentration of the desired fractions in vacuo, a red solid was obtained. UPLC-MS indicated that partial cleavage of the t-butyl ester groups had occurred. The thus obtained mixture (280 mg) was dissolved in a mixture of 1,2-dichloroethane (4 mL) and acetonitrile (2.0 mL). TFA (145 mg, 98 μL, 1.27 mmol) was added and the resulting solution was stirred for 3 h under argon at 0° C. when UPLC-MS indicated that full conversion of the starting material had occurred. The reaction mixture was diluted with 1,2-dichloroethane (4.0 mL) and concentrated at reduced pressure to afford the crude product as a red solid. The crude reaction product was dissolved in MeOH (3 mL) and slowly concentrated at reduced pressure until crystallization started to occur. The crystals were filtered off and washed with Et2O and pentane to afford the title compound as an orange solid. 1H-NMR (400 MHz, DMSO-d6): 12.27 (s, 1H), 8.21 (s, 1H), 7.72-7.66 (m, 2H), 7.58 (d, 1H), 7.40 (d, 1H), 7.14 (t, 1H), 7.02 (t, 1H), 6.65 (t, 1H), 6.24 (d, 1H), 5.34 (d, 2H), 4.14-3.72 (bs, 4H), 3.00-2.73 (bs, 4H), 2.60 (s, 3H). 31P-NMR (162 MHz, DMSO-d6): −2.7. LCMS: [M]+=548.6, Rt(1)=1.72 min., Rt(2)=0.73 min.

Aufarbeitung

  1. concentrationfollowed by concentration at reduced pressure
  2. customThe residue was partitioned between EtOAc
  3. customa saturated aqueous NH4Cl solution, the layers were separated
  4. dry with materialthe organic layer was dried over anhydrous Na2SO4
  5. concentrationConcentration at reduced pressure
  6. customafforded the crude product as a red foam
  7. customThe crude product was purified by reverse phase Gilson HPLC
  8. customAfter concentration of the desired fractions in vacuo, a red solid was obtained
  9. stirringthe resulting solution was stirred for 3 h under argon at 0° C. when UPLC-MS
  10. concentrationconcentrated at reduced pressure
  11. customto afford the crude product as a red solid
  12. customThe crude reaction product
  13. concentrationslowly concentrated at reduced pressure until crystallization
  14. filtrationThe crystals were filtered off
  15. washwashed with Et2O and pentane

Quellen und Nachweise

ORD-Eintrag
ord-29b4629149354c66b50ad711c52ec42e
Quelldatensatz
uspto-grants-2014_04
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US08703782B2

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