HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → 1-[2-(Diphenylmethoxy)ethyl]piperazine
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Benzhydrol | HCID 7037 | — |
| Reactant | 1-(2-Hydroxyethyl)piperazine | HCID 7677 | — |
| Reactant | Bicyclo[2.2.1]heptane-1-methanesulfonic acid, 7,7-dimethyl-2-oxo-, (1S)- | HCID 18462 | — |
| Solvent | Toluene | HCID 1140 | — |
| Product | 1-[2-(Diphenylmethoxy)ethyl]piperazine | HCID 648525 | 24% |
Reaction Steps
In a reactor equipped with a water trap (Dean-Stark trap), a mixture of benzhydrol (5.0 g), 1-(2-hydroxyethyl)piperazine (3.5 g), camphor-10-sulfonic acid (14 g), and toluene (80 mL) was refluxed for 6 hours. Then, 1N-hydrochloric acid was added and the mixture was separated into two phases. The aqueous layer was made basic with 5 N aqueous sodium hydroxide, saturated with sodium chloride, and extracted with chloroform. The extract was washed with a small amount of saturated aqueous NaCl, dried over MgSO4, and concentrated under reduced pressure to provide 1.9 g of the title compound. Yield 24%. This compound was not further purified but directly submitted to the next reaction.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06172085B2 |
| Source dataset | uspto-grants-2001_01 |
| ORD ID | ord-00c1c6630ecf47208eb3f1c7ebf7a44f |
| Source note | uspto-grants-2001_01 |