HuagongsheHuagongshe Chemistry Print Report · For research reference only
Propargyl bromide → 1-Methyl-4-(prop-2-yn-1-yl)piperazine
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Propargyl bromide | HCID 7842 | — |
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | 1-Methylpiperazine | HCID 53167 | — |
| Solvent | Acetone | HCID 180 | — |
| Product | 1-Methyl-4-(prop-2-yn-1-yl)piperazine | HCID 13514091 | — |
Reaction Steps
To 1-methylpiperazine (37.7 ml, 337 mmol) and K2CO3 (46.6 g, 337 mmol) in acetone (380 ml) was added propargyl bromide (25 ml, 225 mmol, 80% in toluene) in acetone (70 ml) dropwise at 0° C. under N2. The internal temperature of the reaction was kept <10° C. The reaction was stirred at room temperature for 3 hours. The reaction was filtered, and the salts were washed with small portions of acetone (×2). The filtrates were combined evaporated to concentration (gently). To the residue was added water and the product was extracted with DCM (×3). The combined organic layers were washed with brine and dried over MgSO4. The product was filtered and evaporated to dryness to yield 1-methyl-4-prop-2-ynyl-piperazine as a yellow oil.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08883790B2 |
| Source dataset | uspto-grants-2014_11 |
| ORD ID | ord-5782530cc31d4ffbad7a8dba200c39de |
| Source note | uspto-grants-2014_11 |