関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 3,6-Dichloropyridazine | HCID 67331 | — |
| 反応物 | 1-Methyl-4-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)-1H-pyrazole | HCID 2773987 | — |
| 触媒 | HCID 178418397 | HCID 178418397 | — |
| 生成物 | 3-Chloro-6-(1-methyl-1H-pyrazol-4-yl)pyridazine | HCID 54595607 | — |
反応手順
In a two-neck flask was placed 3,6-dichloropyridazine (1.49 g, 10 mmol), 1-methylpyrazole-4-boronic acid pinacol ester (1.04 g, 5 mmol), K2CO3 (1.38 g, 10 mmol), and Pd(PPh3)4 (289 mg, 0.25 mmol). The resulting mixture was degassed and refilled with N2 (3 times). 1,4-Dioxane/H2O (9 mL/2 mL) was added and the resulting mixture was heated at 100° C. for 5 h. The resulting mixture was poured into EtOAc/H2O (30 mL/30 mL). The organic layer was washed with brine (30 mL), dried (Na2SO4), and filtered. The solvent was removed and the resulting residue was purified by column using 90-100% EtOAc/hexane as the eluent to yield 3-chloro-6-(1-methyl-1H-pyrazol-4-yl)pyridazine.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US09102669B2 |
|---|
| 出典データセット | uspto-grants-2015_08 |
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| ORD ID | ord-b02337b50d724fa5a9d06b2f50d14bfd |
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| 出典メモ | uspto-grants-2015_08 |
|---|
