Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Acetic Acid | HCID 176 | — |
| Reactant | N,N'-Dimethylethylenediamine | HCID 8070 | — |
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | 1-Benzyl-4-piperidone | HCID 19220 | — |
| Reactant | Sodium Bicarbonate | HCID 516892 | — |
| Reactant | Sodium cyanoborohydride | HCID 5003444 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | HCID 18770447 | HCID 18770447 | 25% |
Reaction Steps
After 1-benzyl-4-piperidone (5.00 g; 26 mmol) and sodium cyanoborohydride (1.25 g; 20 mmol) were added to a solution of N,N′-dimethylethylenediamine (785 mg; 8.9 mmol) in methanol (20 ml) under ice cooling. The ice bath was removed, and acetic acid (2.5 ml; 44 mmol) was added to the solution, and the mixture was stirred for 15 minutes. Potassium carbonate (3 g; 22 mmol) and a saturated aqueous solution of sodium hydrogencarbonate was added to the reaction mixture to conduct extraction with chloroform. The organic layer was washed with saturated brine, dried over anhydrous sodium sulfate and then concentrated under reduced pressure. The resultant crude oil was purified by column chromatography on silica gel, thereby obtaining 955 mg (yield: 25%) of N,N′-bis(1-benzyl-4-piperidinyl)-N,N′-dimethylethylenediamine as a colorless oil.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US06645957B2 |
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| Source dataset | uspto-grants-2003_11 |
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| ORD ID | ord-8d985984869c4cb5b19f4f5d8417119a |
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| Source note | uspto-grants-2003_11 |
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