HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → HCID 21562198, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | 4-Methylbenzaldehyde | HCID 7725 | — |
| Reactant | 2,2,6,6-Tetramethyl-4-piperidone | HCID 13220 | — |
| Reactant | Butyllithium | HCID 178418339 | — |
| Solvent | Diethyl Ether | HCID 3283 | — |
| Solvent | Hexane | HCID 8058 | — |
| Product | HCID 21562198 | HCID 21562198 | — |
Reaction Steps
To a mixture of 12g. of p-tolualdehyde, 15.5 g. of triacetone amine and 50 ml. of anhydrous ether was added dropwise 42.6g. of butyl lithium (as a 15% solution in n-hexane) at -50° to -60°C. under a nitrogen gas stream. After completion of the dropwise addition, the mixture was stirred at room temperature for 3 hours. Then, the reaction mixture was poured into 5% dilute hydrochloric acid with ice-cooling. The aqueous layer was separated and saturated with potassium carbonate. Then, the ether layer was separated and concentrated to yield crude crystalline mass. The mass was recrystallized from benzene to give the desired product as white crystals having a decomposition point of 160° - 161°C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US03933735 |
| Source dataset | uspto-grants-1976_01 |
| ORD ID | ord-5516064907b8436880a5f3e504fefb09 |
| Source note | uspto-grants-1976_01 |