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3-amino-1,1-bis-[3-(3-methoxy-phenyl)-propyl]-piperidinium chloride hydrochloride[ No CAS ]
Yield
Reaction Conditions
Operation in experiment
Example 10 Intermediate 10.1: 3-Amino-1,1-bis-[3-(3-methoxy-phenyl)-propyl]-piperidinium chloride hydrochloride Piperidin-3-yl-carbamic acid tert-butyl ester (110 mg, 0.55 mmol) and 1-(3-Bromo-propyl)-3-methoxy-benzene (320 mg, 1.4 mmol), potassium carbonate (100 mg, 0.72 mmol) and sodium iodide (150 mg, 1 mmol) are dissolved in acetonitril (2 ml) and stirred at reflux overnight and purified by preparative HPLC-MS (MeOH/H2O+0.1% TFA). The residue is dissolved in dichloromethane (1 ml) and TFA (1 ml), stirred at room temperature for 1 h and concentrated in vacuo. The residue is dissolved in acetonitril, 1M HCl (1 ml) is added and evaporated. LC (method L): tR=1.02 min; Mass spectrum (ESI+): m/z=397 [M]+.
Example 10: Intermediate 10.1 : 3-Amino-l,l-bis-[3-(3-methoxy-phenyl)-propyl]-piperidinium chloride hydrochloride Piperidin-3-yl-carbamic acid tert-butyl ester (110 mg, 0.55 mmol) and l-(3-Bromo-propyl)-3-methoxy- benzene (320 mg, 1.4 mmol), potassium carbonate (100 mg, 0.72 mmol) and sodium iodide (150 mg, 1 mmol) are dissolved in acetonitril (2 ml) and stirred at reflux overnight and purified by preparative HPLC-MS (MeOH/H20 + 0.1% TFA). The residue is dissolved in dichloromethane (1 ml) and TFA (1 ml), stirred at room temperature for 1 h and concentrated in vacuo. The residue is dissolved in acetonitril, 1M HCI (1 ml) is added and evaporated. LC (method L): tR = 1.02 min; Mass spectrum (ESI+): m/z = 397 [M]+.
With hydrogenchloride; In ethanol; ethyl acetate; at 50℃; for 5h;
165 g of (R) -piperidine-3-ylcarbamic acid tert-butyl ester (825 mmmol) and 1650 g of ethyl acetate were added to a three-necked reaction flask;500 mL of a hydrochloric acid ethanol solution (5M) was slowly added dropwise at normal temperature; after the drop was completed, the system was raised to 50 C. and reacted for 5 h; the reaction was monitored by TLC.Filtration and drying gave 131 g of R-3-amino-piperidine dihydrochloride (purity: 99%; yield: 92%).
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