HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Benzene, 1-fluoro-2-methyl-4-nitro- → 1-Acetyl-4-(2-methyl-4-nitrophenyl)piperazine
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Benzene, 1-fluoro-2-methyl-4-nitro- | HCID 68001 | — |
| Edukt | 1-Acetylpiperazine | HCID 83795 | — |
| Edukt | 1-Butyl-3-methylimidazolium hexafluorophosphate | HCID 2734174 | — |
| Lösungsmittel | Acetonitrile | HCID 6342 | — |
| Produkt | 1-Acetyl-4-(2-methyl-4-nitrophenyl)piperazine | HCID 5303057 | — |
Reaktionsbedingungen
| Temperatur | 85 °C |
|---|
Reaktionsschritte
1-Butyl-3-methylimidazolium hexafluorophosphate (1.75 g, 7.7 mmol) and acetyl piperazine (39.7 g, 309.4 mmol) was added to a stirred solution of 2-fluoro-5-nitrotoluene (12 g, 77.4 mmol) in MeCN (3 mL) and heated to 85° C. for 2 h. The reaction was cooled and concentrated in vacuo. Water (100 mL) was added to the resulting residue and the reaction extracted with EtOAc (3×100 mL). The solvent was dried (MgSO4), filtered, and concentrated in vacuo to yield the product as a yellow solid which was triturated with isohexane and dried in vacuo at 60° C.; 1H NMR δ 8.05 (2H, m), 7.14 (1H, d), 3.64-3.58 (4H, m), 3.05-2.94 (4H, m), 2.37 (3H, s), 2.37 (3H, s); MS m/e MH+ 264.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US07795283B2 |
| Quelldatensatz | uspto-grants-2010_09 |
| ORD ID | ord-15ead006b72044e7ac3178e63cba7ace |
| Quellennotiz | uspto-grants-2010_09 |