関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Sodium Bicarbonate | HCID 516892 | — |
| 反応物 | 2,6-difluoro-N-[4-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)phenyl]benzamide | HCID 53414211 | — |
| 反応物 | Methyl 4-iodo-5-methylthiophene-2-carboxylate | HCID 59014058 | — |
| 触媒 | Palladium | HCID 23938 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | 4-[4-(2,6-Difluoro-benzoylamino)-phenyl]-5-methyl-thiophene-2-carboxylic acid methyl ester | HCID 24876709 | 12.9% |
反応手順
A mixture of 4-Iodo-5-methyl-thiophene-2-carboxylic acid methyl ester (d, 1 mmol), 2,6-Difluoro-N-[4-(4,4,5,5-tetramethyl-[1,3,2]dioxaborolan-2-yl)-phenyl]-benzamide (c, 1 mmol), palladium catalyst (0.1 mmol), sodium bicarbonate (1 mmol) in a mixture of toluene (5 mL), water (1 mL), ethanol (1 mL) was heated at 100° C. for 24 h. The mixture was taken up with EtOAc (100 mL), washed with water (2×100 mL) and dried (Na2SO4). The oil obtained on concentration was purified by flash chromatography to give 4-[4-(2,6-Difluoro-benzoylamino)-phenyl]-5-methyl-thiophene-2-carboxylic acid methyl ester as a yellowish solid (50 mg).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US08435996B2 |
|---|
| 出典データセット | uspto-grants-2013_05 |
|---|
| ORD ID | ord-c137a143d20840a7ba1a1fd853ece3d9 |
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| 出典メモ | uspto-grants-2013_05 |
|---|
