HuagongsheHuagongshe Chemistry Print Report · For research reference only
Triethylamine → HCID 67663315, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | 1-(2-Pyridyl)piperazine | HCID 94459 | — |
| Reactant | Benzeneacetic acid, alpha-bromo-, methyl ester | HCID 137806 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 67663315 | HCID 67663315 | — |
Reaction Steps
To a solution of racemic α-bromophenylacetic acid methyl ester, 5.0 g (22.0 mmol) in 200 mL of tetrahydrofuran was added 3.4 mL (22.0 mmol) of Et3N and 10 mL (66.0 mmol) of 1-(2-pyridyl)-piperazine. The reaction mixture was refluxed for five hours, cooled to rt. and concentrated to dryness. The residue was partitioned between 20% isopropanol/chloroform and water. The mixture was washed with saturated NaHCO3, washed with brine, dried over Na2SO4, filtered and concentrated to dryness. The residue was purified by column chromatography using MeOH/chloroform as eluant and concentrated to dryness to give a quantitative yield of the desired mixture of isomers as a yellow oil. MS (ion spray) 312.2 (M+).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06743794B2 |
| Source dataset | uspto-grants-2004_06 |
| ORD ID | ord-6a8986e4be8745f9be180d538a3a3c5c |
| Source note | uspto-grants-2004_06 |