Ethyl 4-(1-methylpiperidin-4-ylidenemethyl)-3-trifluoromethylbenzoate → HCID 23145989, Verbindung
Reaktionsgleichung
[CH3:1][N:2]1[CH2:7][CH2:6][C:5](=[CH:8][C:9]2[CH:19]=[CH:18][C:12]([C:13]([O:15][CH2:16][CH3:17])=[O:14])=[CH:11][C:10]=2[C:20]([F:23])([F:22])[F:21])[CH2:4][CH2:3]1>CO.[C].[Pd]>[CH3:1][N:2]1[CH2:3][CH2:4][CH:5]([CH2:8][C:9]2[CH:19]=[CH:18][C:12]([C:13]([O:15][CH2:16][CH3:17])=[O:14])=[CH:11][C:10]=2[C:20]([F:21])([F:23])[F:22])[CH2:6][CH2:7]1Komponenten
4
Edukt 1
Produkt 1
Reagenzien, Katalysatoren, Lösungsmittel 2
Versuchsvorschrift
1.57 g of ethyl 4-(1-methylpiperidin-4-ylidenemethyl)-3-trifluoromethylbenzoate (Reference Example 7 (step 2)) was dissolved in 32 ml of methanol and 78 mg of 10% palladium-carbon was added, and then the mixture was hydrogenated at room temperature under 1 atm for 24 hours. The catalyst was removed by filtration and the solvent in the filtrate was distilled off under reduced pressure. The mixture was again dissolved in 32 ml of methanol and 78 mg of 10% palladium-carbon was added thereto, and then the mixture was hydrogenated at room temperature under 1 atm for 4 hours. Further, 78 mg of palladium-carbon was added and the mixture was hydrogenated at room temperature under 1 atm for 24 hours. 78 mg of palladium-carbon was further added and the mixture was hydrogenated at room temperature under 1 atm for 19 hours. The catalyst was removed by filtration and the solvent in the filtrate was distilled off under reduced pressure to obtain 1.54 g of the objective compound as a green oily product.