Dimethylformamide → HCID 178500174, Verbindung

HRID 1513277Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1513277
OOS([O-])=O.[K+].[CH3:7][O:8][C:9](=[O:24])[C:10]([CH3:23])([CH3:22])[CH2:11][C:12]1[CH:17]=[C:16]([CH3:18])[C:15]([CH:19]=O)=[C:14]([CH3:21])[CH:13]=1.ClC1C=C(N[C:33]2[O:37][C:36]([C:38]3[CH:39]=[CH:40][C:41]4[N:45]=C(C5C(C)=CC(CCC(O)=O)=CC=5C)[NH:43][C:42]=4[CH:59]=3)=[N:35][N:34]=2)C=CC=1.CN([CH:63]=[O:64])C>O>[CH3:7][O:8][C:9](=[O:24])[C:10]([CH3:23])([CH3:22])[CH2:11][C:12]1[CH:17]=[C:16]([CH3:18])[C:15]([C:19]2[NH:45][C:41]3[CH:40]=[CH:39][C:38]([C:36]4[O:37][C:33]([C:12]5[CH:17]=[CH:16][C:15]([O:64][CH3:63])=[CH:14][CH:13]=5)=[N:34][N:35]=4)=[CH:59][C:42]=3[N:43]=2)=[C:14]([CH3:21])[CH:13]=1

Komponenten

6

Edukt 4

HCID 6228DimethylformamideHCID 23707502Potassium hydroxy sulfiteHCID 252105913-(4-{6-[5-(3-Chlorophenylamino)-[1,3,4]oxadiazol-2-yl]-1H-benzoimidazol-2-yl}-3,5-dimethylphenyl)-propionic acidHCID 86632822Methyl 3-(4-formyl-3,5-dimethylphenyl)-2,2-dimethylpropanoate

Produkt 1

HCID 178500174HCID 178500174, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Versuchsvorschrift

Oxone (420 mg, 0.683 mmol) was added to a mixture of 3-(4-formyl-3,5-dimethyl-phenyl)-2,2-dimethyl-propionic acid methyl ester (250 mg, 1.00 mmol) and 4-[5-(4-Methoxy-phenyl)-[1,3,4]oxadiazol-2-yl]-benzene-1,2-diamine (prepared as described in Example 1-59, 300 mg, 1.06 mmol) in DMF (8 mL) and water (0.8 mL), and the mixture was stirred at room temperature for 18 h. The mixture was partitioned between EtOAc and water. The EtOAc extract was washed with brine, dried over Na2SO4, concentrated and chromatographed to give the title compound. m/z 511.3 (MH+).

Aufarbeitung

  1. customThe mixture was partitioned between EtOAc and water
  2. extractionThe EtOAc extract
  3. washwas washed with brine
  4. dry with materialdried over Na2SO4
  5. concentrationconcentrated
  6. customchromatographed

Quellen und Nachweise

ORD-Eintrag
ord-08e483538d34419aa193382d6b9a763a
Quelldatensatz
uspto-grants-2012_07
Patentnummer
US08217065B2

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