HuagongsheHuagongshe Chemistry Print Report · For research reference only
Triethylamine → HCID 66751339, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | 2,2,2-Trichloroethyl chloroformate | HCID 87063 | — |
| Reactant | 1-(2-Tert-butylphenyl)piperazine dihydrochloride | HCID 66751149 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 66751339 | HCID 66751339 | 47% |
Reaction Steps
To an ice-cold mixture of 1-(2-tert-butylphenyl)piperazine dihydrochloride obtained in Reference Example 1 (4.00 g, 3.43 mmol), and triethylamine (4.43 g, 43.8 mmol) in tetrahydrofuran (70 mL) was added 2,2,2-trichloroethyl chloroformate (3.06 g, 14.4 mmol) and the mixture was stirred at room temperature for 48 h. The reaction mixture was partitioned between ethyl acetate and water, and the organic layer was washed with water, saturated brine, dried over anhydrous magnesium sulfate, filtered and concentrated under reduced pressure. The resulting residue was filtered through a pad of silica gel eluted with ethyl acetate to afford a white solid. The solid was triturated with hexane to give the title compound (2.54 g, 47%) as a white solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08853215B2 |
| Source dataset | uspto-grants-2014_10 |
| ORD ID | ord-06883e50da4f4068ba6e900a109df4f2 |
| Source note | uspto-grants-2014_10 |