HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
1-Methylpiperazine → 1-(2-Fluoro-4-iodobenzyl)-4-methylpiperazine
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | 1-Methylpiperazine | HCID 53167 | — |
| Edukt | N-bromobutanimide | HCID 67184 | — |
| Edukt | 2-Fluoro-4-iodotoluene | HCID 123492 | — |
| Lösungsmittel | Ethanol | HCID 702 | — |
| Lösungsmittel | Carbon Tetrachloride | HCID 5943 | — |
| Produkt | 1-(2-Fluoro-4-iodobenzyl)-4-methylpiperazine | HCID 90022493 | 52% |
Reaktionsschritte
To a mixture of 2-fluoro-4-iodotoluene (0.94 g, 4.0 mmol) in CCl4 (40 mL) were added BPO (0.02 g, 0.08 mmol) and NBS (0.78 g, 4.4 mmol) under N2. The reaction mixture was refluxed for 5 h, then cooled and concentrated in vacuo. To the residue was added a solution of methylpiperazine (2.00 g, 20 mmol) in EtOH (40 mL) under N2. The mixture was stirred at rt overnight and concentrated in vacuo. The resulting residue was purified by a silica gel column chromatography (PE/EtOAc (V/V)=10:1) to give the title compound as a white solid (0.69 g, 52%).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US09434695B2 |
| Quelldatensatz | uspto-grants-2016_09 |
| ORD ID | ord-428793b57f3d4fd5afd3cd5b3fa039f4 |
| Quellennotiz | uspto-grants-2016_09 |