HuagongsheHuagongshe Chemistry Print Report · For research reference only
2-Chloro-N-(2-chlorophenyl)acetamide → HCID 69746814, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 2-Chloro-N-(2-chlorophenyl)acetamide | HCID 222444 | — |
| Reactant | Sodium Bicarbonate | HCID 516892 | — |
| Reactant | rel-(2R,6S)-2,6-dimethylpiperazine | HCID 6950261 | — |
| Solvent | Ethanol | HCID 702 | — |
| Product | HCID 69746814 | HCID 69746814 | — |
Reaction Steps
The product of step (i) (5.9 g) was dissolved in ethanol (50 ml) and cis-2,6-dimethylpiperazine (3 g) and sodium hydrogencarbonate (6.63 g) were added at room temperature under a nitrogen atmosphere. The mixture was heated under reflux for 24 hours and the cooled solution was filtered and the filtrate was evaporated under reduced pressure. The residue was dissolved in 1M HCl (22 ml) and washed with dichloromethane. The aqueous solution was then basified to pH13 with a solution of sodium hydroxide and the product was extracted with dichloromethane. The organic layer was washed with water, brine, collected, dried (MgSO4) and concentrated under reduced pressure to give the subtitle compound as a beige solid. Yield 4 g.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06969713B2 |
| Source dataset | uspto-grants-2005_11 |
| ORD ID | ord-b15c0e84c4e4416b9f2b6d0b7a41641c |
| Source note | uspto-grants-2005_11 |