Potassium Carbonate → HCID 22508909, Verbindung

HRID 2111771Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2111771
[F:1][C:2]1[C:10]([O:11][C:12]2[C:17]3=[C:18]([CH3:26])[C:19]([O:21][CH2:22][CH:23]4[CH2:25][O:24]4)=[CH:20][N:16]3[N:15]=[CH:14][N:13]=2)=[CH:9][CH:8]=[C:7]2[C:3]=1[CH:4]=[C:5]([CH3:27])[NH:6]2.[CH3:28][N:29]([CH3:34])[S:30]([NH2:33])(=[O:32])=[O:31].[C:35](=O)([O-])[O-].[K+].[K+]>CN(C=O)C.ClCCl>[F:1][C:2]1[C:10]([O:11][C:12]2[C:17]3=[C:18]([CH3:26])[C:19]([O:21][CH2:22][CH:23]([OH:24])[CH2:25][CH2:35][NH:33][S:30]([N:29]([CH3:34])[CH3:28])(=[O:32])=[O:31])=[CH:20][N:16]3[N:15]=[CH:14][N:13]=2)=[CH:9][CH:8]=[C:7]2[C:3]=1[CH:4]=[C:5]([CH3:27])[NH:6]2

Komponenten

6

Edukt 3

HCID 11430Potassium CarbonateHCID 134472N,N-DimethylsulfamideHCID 22508879HCID 22508879, Verbindung

Produkt 1

HCID 22508909HCID 22508909, VerbindungAusbeute 25 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 6228DimethylformamideLösungsmittelHCID 6344DichloromethaneLösungsmittel

Versuchsvorschrift

A mixture of Example 2 (40 mg, 0.11 mmol), N,N-dimethylsulfamide (94 mg, 0.66 mmol) and potassium carbonate (91 mg, 0.66 mmol) in DMF (0.5 ml) was stirred at 80° C. for 1.5 h. The mixture was diluted with dichloromethane, filtered and concentrated in vacuo. The crude material was purified by preparative HPLC, followed by chromatography on silica gel eluting with 10% methanol in ethyl acetate to afford the title compound (13.7 mg, 25% yield) as a white solid. MS: (M+H)+=493.1

Aufarbeitung

  1. filtrationfiltered
  2. concentrationconcentrated in vacuo
  3. customThe crude material was purified by preparative HPLC

Quellen und Nachweise

ORD-Eintrag
ord-e8697a7bb0c94c56b726b9566f0f50bc
Quelldatensatz
uspto-grants-2009_04
Patentnummer
US07521450B2

Notizen zur Reaktion

Wird geladen…