HuagongsheHuagongshe Chemistry Print Report · For research reference only
Azane;hydrate → HCID 14576908, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Azane;hydrate | HCID 12896473 | — |
| Reactant | HCID 14576878 | HCID 14576878 | — |
| Catalyst | titanium(III) trichloride | HCID 10313229 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | HCID 14576908 | HCID 14576908 | 77% |
Reaction Steps
A solution of 6.5 g of 1-(4-nitrophenyl)-6-(3,4-dichlorophenyl)-2-piperidone in 180 ml of methanol was cooled to 4° C., and then 110 g of 25% titanium trichloride was added dropwise to the solution. After stirring at 18° to 20° C. for 40 minutes, the reaction mixture was poured into cold ammonia water and the precipitates were filtered off. The filtrate was extracted with chloroform. On the other hand, the precipitate obtained above was throughly washed with chloroform. The chloroform layer was combined with the former, washed with water, dried, and concentrated. The residue was recrystallized from ethanol to give 4.59 g of 1-(4-aminophenyl)-6-(3,4-dichlorophenyl)-2-piperidone as colorless prisms.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04839360 |
| Source dataset | uspto-grants-1989_06 |
| ORD ID | ord-93bf49fe32ec4e388042e99a648a2856 |
| Source note | uspto-grants-1989_06 |