Water → HCID 178448116, Verbindung

HRID 1662997Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1662997
[CH:1]([C@H:4]1[CH2:9][CH2:8][C@H:7]([NH:10][C:11]2[C:20]3[C:15](=[CH:16][CH:17]=[CH:18][CH:19]=3)[C:14]([CH2:21][C:22]3[CH:27]=[CH:26][N:25]=[C:24]([O:28]C)[CH:23]=3)=[N:13][N:12]=2)[CH2:6][CH2:5]1)([CH3:3])[CH3:2].C([O-])(O)=O.[Na+].O.CCOC(C)=O>C(Cl)(Cl)Cl.CO>[CH:1]([C@H:4]1[CH2:5][CH2:6][C@H:7]([NH:10][C:11]2[C:20]3[C:15](=[CH:16][CH:17]=[CH:18][CH:19]=3)[C:14]([CH2:21][C:22]3[CH:27]=[CH:26][N:25]=[C:24]([OH:28])[CH:23]=3)=[N:13][N:12]=2)[CH2:8][CH2:9]1)([CH3:3])[CH3:2]

Komponenten

7

Edukt 4

HCID 962WaterHCID 8857Ethyl AcetateHCID 516892Sodium BicarbonateHCID 178489122HCID 178489122, Verbindung

Produkt 1

HCID 178448116HCID 178448116, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 887MethanolLösungsmittelHCID 6212ChloroformLösungsmittel

Reaktionsbedingungen

Temperatur
60 °C

Versuchsvorschrift

Under N2-atmosphere, 0.28 ml (2.05 mMol) Me3Sil are added to 400 mg (1.02 mMol) of trans 1-(4-isopropyl-cyclohexylamino)-4-[2-methoxy-(pyridin-4-yl)-methyl]-phthalazine in 10 ml chloroform, and the resulting mixture is stirred during 20 h at 60° C. After cooling to RT, 5 ml sat. NaHCO3-solution, 5 ml water, 20 ml EtOAc and a small amount of methanol are added, followed by agitation. The resulting white crystals are filtered off, washed with water and dried, yielding the title compound: M.p. 266-267° C. (decomposition); FAB-MS: (M+H)+=377; HPLC(Grad20-100) tRet=10.3). From the filtrate, by extraction with EtOAc, washing of the organic phase with water and brine, drying (Na2SO4), evaporation and crystallisation from dichlormethane/methanol under addition of ether, more product results.

Aufarbeitung

  1. temperatureAfter cooling to RT
  2. filtrationThe resulting white crystals are filtered off
  3. washwashed with water
  4. customdried

Quellen und Nachweise

ORD-Eintrag
ord-27dd13208ff34f13b69d588aaea49572
Quelldatensatz
uspto-grants-2011_10
Patentnummer
US08034814B2

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