HuagongsheHuagongshe Chemistry Print Report · For research reference only
HCID 12833276, compound → 2,4-Dimethyl-5-(1-piperidinyl)benzenamine
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | HCID 12833276 | HCID 12833276 | — |
| Reactant | Aluminium lithium hydride | HCID 21226445 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | 2,4-Dimethyl-5-(1-piperidinyl)benzenamine | HCID 13062336 | — |
Reaction Steps
6.2 g of lithium aluminium hydride are introduced into 200 ml of absolute tetrahydrofuran. 26 g (0.12 mol) of 1-(3'-amino-4',6'-dimethylphenyl)-piperidin-2-one are added in portions, with stirring. The mixture is then refluxed for 1 hour. Excess LiAlH4 is destroyed with ethyl acetate. 2 N Hcl is added to the mixture until the pH is 4-5, ether is added and the mixture is extracted twice with 2 N KOH solution. The organic phase is washed with water and saturated NaCl solution, dried with MgSO4, clarified with active charcoal and evaporated. The residue is distilled in a bulb tube. This gives 18.2 g (73%) of a yellow oil (boiling point 140°/0.001 mm Hg).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04294606 |
| Source dataset | uspto-grants-1981_10 |
| ORD ID | ord-6523d336c32147acb589d32f1f061f72 |
| Source note | uspto-grants-1981_10 |