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Triethylamine → 5-((4-(4-Amino-3-fluorobenzoyl)piperazin-1-yl)methyl)-N-tert-butylfuran-2-carboxamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | 4-Amino-3-fluorobenzoic acid | HCID 9971 | — |
| 反応物 | Propylphosphonic anhydride | HCID 111923 | — |
| 反応物 | N-tert-butyl-5-(piperazin-1-ylmethyl)furan-2-carboxamide | HCID 66661240 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 5-((4-(4-Amino-3-fluorobenzoyl)piperazin-1-yl)methyl)-N-tert-butylfuran-2-carboxamide | HCID 66661523 | 40.6% |
反応手順
To a solution of 4-amino-3-fluorobenzoic acid (0.883 g, 5.69 mmol), N-tert-butyl-5-(piperazin-1-ylmethyl)furan-2-carboxamide (1.51 g, 5.69 mmol) and triethyl-amine (0.576 g, 5.69 mmol, 0.791 mL) in dichloromethane was added 1-propanephosphonic acid cyclic anhydride (3.62 g, 5.69 mmol, 3.39 mL, 50% solution in ethyl acetate). The reaction was stirred for 2 hours then concentrated under reduced pressure. The residue was taken up in ethyl acetate, washed with sodium bicarbonate, water and brine. The organic phase was concentrated under reduced pressure to give the title compound (0.93 g). MS (ESI) m/z 403.6 [M+H]+
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08759352B2 |
| 出典データセット | uspto-grants-2014_06 |
| ORD ID | ord-9cc62522761947f9889e7d087f48d5f3 |
| 出典メモ | uspto-grants-2014_06 |