HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Triethylamine → 1-(2-Chloro-4-nitrobenzyl)-4-methylpiperazine
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Triethylamine | HCID 8471 | — |
| Edukt | 1-Methylpiperazine | HCID 53167 | — |
| Edukt | Sodium Bicarbonate | HCID 516892 | — |
| Edukt | 1-(Bromomethyl)-2-chloro-4-nitrobenzene | HCID 3016368 | — |
| Lösungsmittel | Dichloromethane | HCID 6344 | — |
| Produkt | 1-(2-Chloro-4-nitrobenzyl)-4-methylpiperazine | HCID 66735814 | 86,6% |
Reaktionsschritte
To a solution of crude 1-(bromomethyl)-2-chloro-4-nitro-benzene (29.1 mmol; 50% pure) in 30 mL of DCM was added Et3N (4.2 mL, 30 mmol) and 1-methylpiperazine (3.4 mL, 30 mmol). After stirring for 3 h at ambient temperature, aq. NaHCO3 was added and the mixture was extracted with DCM. The combined organic layer was dried over Na2SO4, filtered, concentrated, and the resulting residue was purified by silica gel chromatography (eluted with 5% MeOH/DCM) to provide 6.80 g of product as a dark yellow oil.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US09029533B2 |
| Quelldatensatz | uspto-grants-2015_05 |
| ORD ID | ord-6437dee56f534ba69acbb49c8b5920b1 |
| Quellennotiz | uspto-grants-2015_05 |