HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Oxalyl chloride → 2-Methylcyclohexanecarbonyl chloride
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Oxalyl chloride | HCID 65578 | — |
| Edukt | 2-Methylcyclohexanecarboxylic acid | HCID 85811 | — |
| Katalysator | Dimethylformamide | HCID 6228 | — |
| Lösungsmittel | Dichloromethane | HCID 6344 | — |
| Produkt | 2-Methylcyclohexanecarbonyl chloride | HCID 2759837 | 102,3% |
Reaktionsschritte
To a solution of 2-methylcyclohexanecarboxylic acid (6.00 mL, 42.6 mmol, mixture of cis and trans) in DCM (60 mL) was added oxalyl chloride (4.80 mL, 55.3 mmol) followed by DMF (0.03 mL, 0.4 mmol). The reaction mixture was stirred at ambient temperature for about 4 h before it was concentrated under reduced pressure to constant weight to afford 2-methylcyclohexanecarbonyl chloride (mixture of diastereomers) as a yellow oil (7.0 g, 97%): 1H NMR (400 MHz, CDCl3) δ 2.98-2.94 (m, 1H), 2.39-2.35 (m, 1H), 1.91-1.82 (m, 1H), 1.79-1.72 (m, 1H), 1.69-1.60 (m, 2H), 1.57-1.47 (m, 2H), 1.42-1.36 (m, 1H), 1.34-1.26 (m, 1H), 1.04-0.96 (m, 3H).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US09365579B2 |
| Quelldatensatz | uspto-grants-2016_06 |
| ORD ID | ord-53637888526143f384cf31a59bb0de1c |
| Quellennotiz | uspto-grants-2016_06 |