HuagongsheHuagongshe Chemistry Print Report · For research reference only
Triethylamine → HCID 66750875, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Ethoxalyl chloride | HCID 20884 | — |
| Reactant | HCID 66750915 | HCID 66750915 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 66750875 | HCID 66750875 | 90.2% |
Reaction Steps
To a mixture of 1-(2-tert-butyl-4-chlorophenyl)piperazine dihydrochloride (Reference Example 20, 0.50 g, 1.54 mmol) and triethylamine (0.48 g, 4.77 mmol) in THF (30 mL) was added ethyl chloro(oxo)acetate (0.23 g, 1.69 mmol). The mixture was stirred at room temperature for 1 h, filtered and concentrated under reduced pressure. The resulting residue was partitioned between ethyl acetate and water. The organic layer was washed with saturated brine, died over anhydrous magnesium sulfate, filtered and concentrated under reduced pressure. The resulting residue was purified by flash column chromatography (silica gel, 9:1-3:7, hexane/ethyl acetate) to give the title compound (0.49 g) as a colorless solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08853215B2 |
| Source dataset | uspto-grants-2014_10 |
| ORD ID | ord-6d6493baa13c4096a918feb581e11bcc |
| Source note | uspto-grants-2014_10 |