HuagongsheHuagongshe Chemistry Print Report · For research reference only
Triethylamine → HCID 66559508, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | 3-Bromobenzyl bromide | HCID 69979 | — |
| Reactant | 1-(2,3-Dichlorophenyl)piperazine hydrochloride | HCID 11630372 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Acetonitrile | HCID 6342 | — |
| Product | HCID 66559508 | HCID 66559508 | 74% |
Reaction Steps
A mixture of 1-(2,3-dichlorophenyl)piperazine hydrochloride (intermediate 41) (294 mg, 1.1 mmol), 1-bromo-3-(bromomethyl)benzene (250 mg, 1 mmol) and anhydrous triethylamine (253 mg, 2.5 mmol) was dissolved in CH3CN and the solution was heated to reflux for 4 h. The solution was diluted with water and extracted with EtOAc. The combined organic layers were washed with saturated aq NaHCO3, brine, dried over anhydrous Na2SO4, concentrated in vacuo and purified by flash chromatography on silica gel column (elution with PE/EtOAc=8:1) to give 1-(3-bromobenzyl)-4-(2,3-dichlorophenyl)piperazine (intermediate 53) (220 mg, 74%) as a white solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09156822B2 |
| Source dataset | uspto-grants-2015_10 |
| ORD ID | ord-524f8eee58e34a8ea4c6db96c177da2f |
| Source note | uspto-grants-2015_10 |