HuagongsheHuagongshe Chemistry Print Report · For research reference only
Dichloromethane → 1-[4-Bromo-2-(4,4-dimethylcyclohexyl)phenyl]piperazine
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Dichloromethane | HCID 6344 | — |
| Reactant | Trifluoroacetic acid | HCID 6422 | — |
| Reactant | Sodium Carbonate | HCID 10340 | — |
| Reactant | 4-[4-Bromo-2-(4,4-dimethylcyclohexyl)phenyl]piperazine-1-carboxylic acid t-butyl ester | HCID 59769418 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | 1-[4-Bromo-2-(4,4-dimethylcyclohexyl)phenyl]piperazine | HCID 23142089 | 103.7% |
Reaction Steps
A mixture of 4-[4-bromo-2-(4,4-dimethylcyclohexyl)phenyl]piperazine-1-carboxylic acid t-butyl ester (1.5 g, 3.32 mmol) produced in Example (3e), trifluoroacetic acid (3 mL, 38.7 mmol) and dichloromethane (6 mL) was stirred for 2 hours and 30 minutes at room temperature. Saturated aqueous solution of sodium carbonate was added to the reaction mixture and extraction was performed with ethyl acetate. The separated organic layer was washed with water and brine in that order and then dried over anhydrous sodium sulfate. The desiccant was filtered off and the filtrate was concentrated under reduced pressure. The residue was dried under reduced pressure to give 1.21 g of a crude product of the title compound as a brown oil.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07425554B2 |
| Source dataset | uspto-grants-2008_09 |
| ORD ID | ord-369d6936f64943aba1f9b932445c8d80 |
| Source note | uspto-grants-2008_09 |