Reaktionsgleichung
[CH3:1][O:2][C:3]1[CH:4]=[C:5]([CH2:11][C:12]([OH:14])=O)[CH:6]=[C:7]([O:9][CH3:10])[CH:8]=1.C(N1[CH:26]=[CH:25]N=C1)(N1C=CN=C1)=O.C[NH:28][C:29]1[C:30]([C:35]2[CH:40]=[C:39]([N:41]3[CH2:46][CH2:45][O:44][CH2:43][CH2:42]3)[C:38]([CH3:47])=[CH:37][CH:36]=2)=[N:31][CH:32]=CC=1.[CH3:48]N(C)C=O>>[CH3:10][O:9][C:7]1[CH:6]=[C:5]([CH2:11][C:12]([N:31]([CH3:32])[C:30]2[CH:29]=[N:28][C:39]([N:41]3[CH2:42][CH2:43][O:44][CH2:45][CH2:46]3)=[CH:40][C:35]=2[C:36]2[CH:37]=[CH:38][CH:47]=[CH:48][C:25]=2[CH3:26])=[O:14])[CH:4]=[C:3]([O:2][CH3:1])[CH:8]=1Komponenten
5
Versuchsvorschrift
To a solution of 226 mg (1.15 mmol) 3,5-dimethoxy-phenylacetic acid in 7 ml N,N-dimethylformamide were added 244 mg (1.5 mmol) 1,1′-carbonyl-diimidazole and the solution was stirred for 30 min at room temperature. After addition of 283 mg (1 mmol) of methyl-(6-morpholin-4-yl-4-tolyl-pyridin-3-yl)-amine (as described in step f) for the preparation of Example 23), the reaction mixture was heated at 70° C. for 7 h. After cooling to room temperature, the solvent was removed in vacuo and the residue was re-dissolved in 30 ml ethyl acetate. The organic phase was washed with water (2×30 ml), brine, dried (magnesium sulfate) and evaporated. Flash chromatography gave 347 mg (75%) of the title compound as a white foam.
Aufarbeitung
- customfor the preparation of Example 23), the reaction mixture
- temperaturewas heated at 70° C. for 7 h
- temperatureAfter cooling to room temperature
- customthe solvent was removed in vacuo
- dissolutionthe residue was re-dissolved in 30 ml ethyl acetate
- washThe organic phase was washed with water (2×30 ml), brine
- dry with materialdried (magnesium sulfate)
- customevaporated
Quellen und Nachweise
- ORD-Eintrag
- ord-867d8a06ea764c1f8bb01de3cf201f27
- Quelldatensatz
- uspto-grants-2001_10
- Patentnummer
- US06297375B1
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