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Trichloroacetyl isocyanate → Methyl 2-({[(trichloroacetyl)amino]carbonyl}amino)thiophene-3-carboxylate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Trichloroacetyl isocyanate | HCID 76400 | — |
| 反応物 | Methyl 2-amino-3-thenoate | HCID 78381 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | Methyl 2-({[(trichloroacetyl)amino]carbonyl}amino)thiophene-3-carboxylate | HCID 59789494 | — |
反応手順
To a stirred solution of 2-amino-thiophene-3-carboxylic acid methyl ester (1 eq) in anhydrous THF (mL) was added trichloroacetyl isocyanate (1 eq) slowly over a period of 5 min. After the addition was complete, a precipitate formed and the reaction stirred for an additional 1 h. The desired product was obtained by filtration to give methyl 2-({[(trichloroacetyl)amino]carbonyl}amino)thiophene-3-carboxylate (99%) as an off-white solid. The product was used in the next step without any further purification. LC/MS (ES, M+H=345).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07423061B2 |
| 出典データセット | uspto-grants-2008_09 |
| ORD ID | ord-c9ad578238324991a9f7cd8df5c4dd1c |
| 出典メモ | uspto-grants-2008_09 |