HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Propylamine → 2,6-difluoro-N-vinyl-benzamide
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Propylamine | HCID 7852 | — |
| Edukt | 2,6-difluoro-N-formyl-N-vinyl-benzamide | HCID 89760769 | — |
| Lösungsmittel | Dichloromethane | HCID 6344 | — |
| Produkt | 2,6-difluoro-N-vinyl-benzamide | HCID 89760782 | 75% |
Reaktionsschritte
n-Propylamine (36.7 ml, 26.33 g, 444 mmol) was added to a solution of crude 2,6-difluoro-N-formyl-N-vinyl-benzamide from step a (47 g, 222 mmol) in dichloromethane (200 ml). There was a weak exotherm. The reaction mixture was kept at room temperature with a cold water bath. The solution was then concentrated on the rotovap to give a brown oil, which was crystallised from ethanol/water to yield 30 g (75%) of pure 2,6-difluoro-N-vinyl-benzamide as beige crystals. A further 5.7 g was crystallised from concentration of the mother liquors. M.p. 103-107° C.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US09408392B2 |
| Quelldatensatz | uspto-grants-2016_08 |
| ORD ID | ord-0ebfbf5bc9024a329865b68ac8740637 |
| Quellennotiz | uspto-grants-2016_08 |