HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Dimethylamine → 2-chloro-4,5-difluoro-N,N-dimethylbenzamide
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Dimethylamine | HCID 674 | — |
| Edukt | Tetrahydrofuran | HCID 8028 | — |
| Edukt | Triethylamine | HCID 8471 | — |
| Edukt | 1-Chloro-N,N-2-trimethylpropenylamine | HCID 640792 | — |
| Edukt | 2-Chloro-4,5-difluorobenzoic acid | HCID 737171 | — |
| Lösungsmittel | Hydrochloric Acid | HCID 313 | — |
| Lösungsmittel | Dichloromethane | HCID 6344 | — |
| Produkt | 2-chloro-4,5-difluoro-N,N-dimethylbenzamide | HCID 59346904 | 96,8% |
Reaktionsschritte
A solution of 2-chloro-4,5-difluorobenzoic acid (385 mg, 2.0 mmol) in DCM (5 mL) was treated with (1-chloro-2-methylprop-1-en-1-yl)dimethylamine (293 mg, 2.2 mmol) and stirred under argon for 1 hour. The mixture was then treated with triethylamine (0.56 mL, 4.0 mmol) and a 2M solution of dimethylamine in THF (1.2 mL, 2.4 mmol), and stirred for 18 hours. The mixture was diluted with DCM (5 mL) and 2M hydrochloric acid (4 mL) and separated. The organic layer was dried (MgSO4), filtered and concentrated in vacuo to afford the title compound (425 mg). The residue was used without further purification.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US07745475B2 |
| Quelldatensatz | uspto-grants-2010_06 |
| ORD ID | ord-29d4985e8b5643428721490fac721520 |
| Quellennotiz | uspto-grants-2010_06 |