O=C1CNCCN1.[CH2:8]([N:10]([CH2:26][CH3:27])[CH:11]([N:13]1[CH2:18][CH2:17][NH:16][C:15](=O)[CH:14]1[C:20]1[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=1)[CH3:12])[CH3:9].O1CCOCC1.[OH-].[Na+]>O.CCOCC>[CH2:26]([N:10]([CH2:8][CH3:9])[CH:11]([N:13]1[CH2:18][CH2:17][NH:16][CH2:15][CH:14]1[C:20]1[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=1)[CH3:12])[CH3:27]
89 g. of the keto piperazine prepared as described hereinabove under (a), are dissolved in 200 cc. of absolute dioxane. The solution is added to a suspension of 20 g. of lithium aluminum hydride LiAlH4 in 800 cc. of absolute ether while exposing the mixture to vibration. After addition of the keto piperazine solution is completed, the reaction mixture is boiled under reflux for 6 hours. Thereafter it is decomposed by successive treatment with 21 cc. of 15 % sodium hydroxide solution, 21 cc. of water, 63 cc. of 15 % sodium hydroxide solution, and 42 cc. of water. The decomposed reaction mixture is filtered, the solvent is removed by distillation, and the residue is distilled in a vacuum. 65 g. of a light yellow oil of the boiling point 114°-117° C./0.05 mm. Hg are obtained. This oil corresponds to the above given compound. The yield is 77 % of the theoretical yield.
Wird geladen…
