Reaktionsgleichung
[CH3:1][C@H:2]1[CH2:7][CH2:6][C@H:5]([NH:8][C:9](=O)[CH2:10][N:11]([CH3:13])[CH3:12])[CH2:4][CH2:3]1.[H-].[Al+3].[Li+].[H-].[H-].[H-].O.O.O.O.O.O.O.O.O.O.S([O-])([O-])(=O)=O.[Na+].[Na+]>C1COCC1>[CH3:12][N:11]([CH3:13])[CH2:10][CH2:9][NH:8][C@H:5]1[CH2:4][CH2:3][C@H:2]([CH3:1])[CH2:7][CH2:6]1Komponenten
Edukt 3
Produkt 1
Reagenzien, Katalysatoren, Lösungsmittel 1
Versuchsvorschrift
8.5 g of N-(trans-4-methylcyclohexyl)-2-dimethylaminoacetamide was dissolved in 100 ml of THF. Under an argon stream, the solution was added dropwise to a solution of 3.6 g of lithium aluminum hydride suspended in 200 ml of THF under ice-cooling. After the addition, the solution was reacted for 8 hours, while it was refluxed. After reaction, the solution was allowed to cool to room temperature. Then, 10 g of sodium sulfate decahydrate was added to the solution under ice-cooling. The solution was stirred for 1 hour, and the precipitate was filtered out. The solvent was removed in vacuo to obtaine an oily substance. This substance was refined by vacuum distillation, yielding 3.8 g of N-(2-dimethylaminoethyl)-trans-4-methylcyclohexylamine as a colorless oil, which had the following physiochemical properties:
Aufarbeitung
- temperaturecooling
- additionAfter the addition
- customthe solution was reacted for 8 hours, while it
- temperaturewas refluxed
- customAfter reaction
- temperaturecooling
- filtrationthe precipitate was filtered out
- customThe solvent was removed in vacuo
- distillationThis substance was refined by vacuum distillation
Quellen und Nachweise
- ORD-Eintrag
- ord-a98b033b1a784888b2a2f4a3155cd5d6
- Quelldatensatz
- uspto-grants-1994_09
- Patentnummer
- US05344845
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