関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Methyl iodide | HCID 6328 | — |
| 反応物 | Cesium carbonate | HCID 10796 | — |
| 反応物 | 6-Chloropyridazin-3-ol | HCID 252828 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 生成物 | 6-Chloro-2-methyl-2,3-dihydropyridazin-3-one | HCID 2783607 | 749.4% |
反応手順
To a solution of 6-chloropyridazin-3(2H)-one (780 mg, 6 mmol) in CH3CN (40 mL) was added Cs2CO3 (3.9 g, 12 mmol) and CH3I (1 mL, 12 mmol) and the reaction mixture was stirred at 70° C. overnight. Solid was removed by filtration and the filtrate was concentrated under reduced pressure. The residue was purified by silica gel chromatography (hexane/EA=3/1) to afford the title compound as orange oil (6.5 g, 75%). [LCMS: Rt=1.43 min, m/z 145.1 (M+H)+].
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US09273026B2 |
|---|
| 出典データセット | uspto-grants-2016_03 |
|---|
| ORD ID | ord-7997c72e78a14be2a72752afc37afc7e |
|---|
| 出典メモ | uspto-grants-2016_03 |
|---|
