Ethanol → (4-(Dimethylamino)butyl)(methyl)amine
反応式
[H-].[Al+3].[Li+].[H-].[H-].[H-].[CH3:7][N:8]([CH3:16])[CH2:9][CH2:10][CH2:11][CH2:12][NH:13][CH:14]=O.C(O)C>C1COCC1>[CH3:7][N:8]([CH3:16])[CH2:9][CH2:10][CH2:11][CH2:12][NH:13][CH3:14][H-].[Al+3].[Li+].[H-].[H-].[H-].[CH3:7][N:8]([CH3:16])[CH2:9][CH2:10][CH2:11][CH2:12][NH:13][CH:14]=O.C(O)C>C1COCC1>[CH3:7][N:8]([CH3:16])[CH2:9][CH2:10][CH2:11][CH2:12][NH:13][CH3:14]A solution of lithium aluminium hydride in THF (1M, 28 mL) was added dropwise to a stirred, cooled solution of N-(4-dimethylaminobutyl)formamide (Intermediate 79, 2.7 g) in THF (60 mL) while maintaining the temperature at 0° C. under an atmosphere of nitrogen. On completion of the addition, the mixture was stirred and heated at 75° C. for 2 hours. The reaction mixture was cooled to 0° C. and ethanol was added then the mixture was evaporated to dryness. The residue was diluted with a mixture of diethyl ether and DCM (30%) and the solid was filtered off. The filtrate was evaporated to dryness to give N-(4-dimethylaminobutyl)-N-methylamine (1.5 g) as a yellow oil.
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