関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Sodium Carbonate | HCID 10340 | — |
| 反応物 | 3,6-Dichloropyridazine | HCID 67331 | — |
| 反応物 | p-Chlorophenylboric acid | HCID 17810664 | — |
| 触媒 | Bis(cyclopenta-1,4-dien-1-yl(diphenyl)phosphane);dichloropalladium;iron(2+) | HCID 178418228 | — |
| 溶媒 | 1,4-Dioxane | HCID 31275 | — |
| 生成物 | 3-Chloro-6-(4-chlorophenyl)pyridazine | HCID 12257502 | — |
反応手順
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).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US07452911B2 |
|---|
| 出典データセット | uspto-grants-2008_11 |
|---|
| ORD ID | ord-58f9c3b7b7de47869439a62f3987251e |
|---|
| 出典メモ | uspto-grants-2008_11 |
|---|
