2-Amino-1-[4-(3,4-dichlorophenoxy)-piperidine-1-yl]-3-methyl-butan-1-one → 1-[4-(3,4-Dichlorophenoxy)-piperidin-1-ylmethyl]-2-methyl-propylamine
Reaktionsgleichung
[NH2:1][CH:2]([CH:20]([CH3:22])[CH3:21])[C:3]([N:5]1[CH2:10][CH2:9][CH:8]([O:11][C:12]2[CH:17]=[CH:16][C:15]([Cl:18])=[C:14]([Cl:19])[CH:13]=2)[CH2:7][CH2:6]1)=O>C1COCC1>[Cl:19][C:14]1[CH:13]=[C:12]([CH:17]=[CH:16][C:15]=1[Cl:18])[O:11][CH:8]1[CH2:7][CH2:6][N:5]([CH2:3][CH:2]([NH2:1])[CH:20]([CH3:21])[CH3:22])[CH2:10][CH2:9]1Komponenten
3
Edukt 1
Produkt 1
Reagenzien, Katalysatoren, Lösungsmittel 1
Reaktionsbedingungen
- Temperatur
- 70 °C
Versuchsvorschrift
The product of step (ii) (1.12 g) was dissolved in THF (10 ml) and Borane/THF complex (22.7 ml) added. The mixture was heated under reflux for 2 hours and cooled. The solvent was evaporated, the product dissolved in methanol (5 ml) and 50% aqueous HCl solution added. The mixture was heated to 70° C. for 1 hour and cooled to room temperature. The solvent was removed, ethyl acetate and 2N aqueous NaOH solution were added to give pH 9.0. The organic phase was separated and the solvent evaporated to give the sub-titled compound as an oil (0.98 g) which used without further purification.
Aufarbeitung
- additionBorane/THF complex (22.7 ml) added
- temperatureThe mixture was heated
- temperatureunder reflux for 2 hours
- temperaturecooled
- customThe solvent was evaporated
- dissolutionthe product dissolved in methanol (5 ml)
- addition50% aqueous HCl solution added
- temperaturecooled to room temperature
- customThe solvent was removed
- additionethyl acetate and 2N aqueous NaOH solution were added
- customto give pH 9.0
- customThe organic phase was separated
- customthe solvent evaporated
Quellen und Nachweise
- ORD-Eintrag
- ord-3ca421c901c242289dc465b17f7c8c6f
- Quelldatensatz
- uspto-grants-2005_09
- Patentnummer
- US06946478B2
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