化工社化工社 化学情報印刷レポート · 研究参考用
Triethylamine → N-(6-fluoro-1,3-benzothiazol-2-yl)-2,2,3,3-tetramethylcyclopropanecarboxamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | 1-Hydroxybenzotriazole | HCID 75771 | — |
| 反応物 | 2,2,3,3-Tetramethylcyclopropanecarboxylic acid | HCID 152115 | — |
| 反応物 | 2-Amino-6-fluorobenzothiazole | HCID 319954 | — |
| 反応物 | 1,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochloride | HCID 2723939 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 溶媒 | Triethylamine tetrahydrofuran | HCID 68616177 | — |
| 生成物 | N-(6-fluoro-1,3-benzothiazol-2-yl)-2,2,3,3-tetramethylcyclopropanecarboxamide | HCID 86618903 | — |
反応手順
A mixture of 6-fluoro-benzothiazol-2-ylamine (1 equiv), N-(3-dimethylaminopropyl)-N-ethylcarbodiimide hydrochloride (1 equiv), 1-hydroxybenzotriazole, triethylamine (1.1 equiv), and 2,2,3,3-tetramethylcyclopropanecarboxylic acid (0.8 equiv) in 3:1 THF/Et3N (1 M) and were stirred overnight at room temperature. The mixture was diluted with EtOAc, washed with 1 M aqueous NaHCO3, dried (Na2SO4), filtered, and concentrated. Puried by silica gel chromatography afforded the title compound. MS (ESI+) m/z 293 (M+H)+.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08841334B2 |
| 出典データセット | uspto-grants-2014_09 |
| ORD ID | ord-34bf5f0fff8949ce9fdf3d6afcec3606 |
| 出典メモ | uspto-grants-2014_09 |