関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 1-Methyl-5-(tributylstannyl)-1H-pyrazole | HCID 21867455 | — |
| 反応物 | 2-Amino-4-difluoromethyl-5-iodo-benzoic acid methyl ester | HCID 59164445 | — |
| 触媒 | HCID 178418476 | HCID 178418476 | — |
| 溶媒 | 1,4-Dioxane | HCID 31275 | — |
| 生成物 | HCID 59164478 | HCID 59164478 | 31.1% |
反応手順
To a solution of 2-amino-4-difluoromethyl-5-iodo-benzoic acid methyl ester (750 mg, 2.29 mmol) in dioxane (30 mL) were added 1-methyl-5-tributylstannanyl-1H-pyrazole (1.28 g, 1.5 equiv) and Pd(PPh3)2Cl2 (246 mg, 0.15 equiv) and the resulting mixture was stirred at 90° C. for 18 h. The solvent was removed in vacuo to afford a dark oil. The crude product was purified by flash chromatography (silica gel, EtOAc/hexanes (0:100 to 50:50)) to provide the title compound as a yellow oil (200 mg, 31%). ES-MS: m/z 282.3 [M+H]+, rt 4.97 min.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US08012988B2 |
|---|
| 出典データセット | uspto-grants-2011_09 |
|---|
| ORD ID | ord-c2028ae3ddd443919a0cde5eb216726d |
|---|
| 出典メモ | uspto-grants-2011_09 |
|---|
