Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|
| Edukt | Water | HCID 962 | — |
| Edukt | Sodium Carbonate | HCID 10340 | — |
| Edukt | 3,6-Dichloropyridazine | HCID 67331 | — |
| Edukt | p-Chlorophenylboric acid | HCID 17810664 | — |
| Katalysator | Bis(cyclopenta-1,4-dien-1-yl(diphenyl)phosphane);dichloropalladium;iron(2+) | HCID 178418228 | — |
| Lösungsmittel | 1,4-Dioxane | HCID 31275 | — |
| Produkt | 3-Chloro-6-(4-chlorophenyl)pyridazine | HCID 12257502 | — |
Reaktionsschritte
Under an argon atmosphere a solution of 11.3 g (70.5 mmol) 4-chlorophenylboric acid in 50 mL 1,4-dioxane is added to a solution of 10.8 g (70.5 mmol) 3,6-dichloropyridazine, 10 mL (20 mmol) of a 2 M Na2CO3 solution and 600 mg (0.73 mmol) Pd(dppf)Cl2 in 150 mL 1,4-dioxane at 110° C. over 2 h. The reaction mixture is stirred for 1 h at 110° C. 100 mL water are added and the aqueous phase is extracted with 100 mL EtOAc. The organic phase is dried over Na2SO4 and the solvent is eliminated i.vac. Purification is carried out by column chromatography on silica gel (cyc/EtOAc 4:1).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| Patentnummer | US07452911B2 |
|---|
| Quelldatensatz | uspto-grants-2008_11 |
|---|
| ORD ID | ord-58f9c3b7b7de47869439a62f3987251e |
|---|
| Quellennotiz | uspto-grants-2008_11 |
|---|
