HuagongsheHuagongshe Chemistry Print Report · For research reference only
1,3-Dibromobenzene → 1-(3-Bromophenyl)-4-methylpiperazine
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 1,3-Dibromobenzene | HCID 7927 | — |
| Reactant | 1-Methylpiperazine | HCID 53167 | — |
| Solvent | tert-Butyl methyl ether | HCID 15413 | — |
| Product | 1-(3-Bromophenyl)-4-methylpiperazine | HCID 53415329 | — |
Reaction Steps
1-Methyl-piperazine (1 ml, 8.99 mmol) and 1,3-dibromo-benzene (3 ml, 24.82 mmol) are heated to 200° C. in a sealed tube under microwave irradiation for 300 min (150 W, 9 bar). The residue is diluted with tert-butyl methyl ether (50 ml) and extracted with 1M HCl. The aqueous layer is neutralized with sodium bicarbonate, and extracted with ethyl acetate (150 ml). The organic layer is separated and dried over MgSO4. The drying agent is filtered and the solvent is removed in vacuum; yield: 700 mg 1-(3-bromo-phenyl)-4-methyl-piperazine; HPLC/MS: 1.24 min, [M+H]=255.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09045493B2 |
| Source dataset | uspto-grants-2015_06 |
| ORD ID | ord-3348b72d8d484cce8e211e55b78f59cb |
| Source note | uspto-grants-2015_06 |