Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Sulfuric Acid | HCID 1118 | — |
| Reactant | Aluminium lithium hydride | HCID 21226445 | — |
| Reactant | 1-Methyl-4-phenylpiperidine-4-carbonitrile--hydrogen chloride (1/1) | HCID 24885960 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 68707356 | HCID 68707356 | — |
Reaction Steps
To a solution of LAH (7.5 mmol) in THF (10 mL) is added dropwise conc. H2SO4 (3.8 mmol) at 0° C. After stirred at 0° C. for 0.5 h, 1-methyl-4-phenylpiperidine-4-carbonitrile hydrochloride (2.5 mmol) is added at 0° C. The reaction mixture is stirred at 60° C. for 6 h. After cooled down to 0° C., the reaction is quenched by the addition of Na2SO4-10H2O. The resulting mixture is filtered through celite, and the filtrate is concentrated in vacuo. The residue is suspended in ether and treated with HCl in 1,4-dioxane. The resulting white solid is collected by filtration to give the title compound, which is directly used for the next reaction without further purification.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US07704996B2 |
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| Source dataset | uspto-grants-2010_04 |
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| ORD ID | ord-7317d27a5b354a7994047732e0940f02 |
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| Source note | uspto-grants-2010_04 |
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