関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | Thionyl Chloride | HCID 24386 | — |
| 反応物 | Pyrrolidine | HCID 31268 | — |
| 反応物 | 3-Fluoro-4-nitrobenzoic acid | HCID 230653 | — |
| 触媒 | Dimethylformamide | HCID 6228 | — |
| 溶媒 | Benzene | HCID 241 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | (3-Fluoro-4-nitro-phenyl)-pyrrolidin-1-yl-methanone | HCID 55103417 | — |
反応手順
1.00 g (5.40 mmol) 3-Fluoro-4-nitro-benzoic acid were suspended in 55 mL benzene. 1 mL Thionyl chloride and 7 drops DMF were added. The resulting mixture was stirred of 5 h at 70° C. and then concentrated under reduced pressure. The residue was dissolved in 40 mL CH2Cl2. Subsequently 0.75 mL (5.40 mmol) triethylamine and 0.45 mL (5.40 mmol) pyrrolidine were added and the resulting solution was stirred for 1 h at room temperature. The mixture was diluted with CH2Cl2 and washed subsequently with a 0.1 N HCl-solution, with a saturated NaHCO3-solution and with brine. The organic layer was dried over anhydrous MgSO4 and concentrated under vacuo to give crude (3-Fluoro-4-nitro-phenyl)-pyrrolidin-1-yl-methanone as an orange solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07741341B2 |
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| 出典データセット | uspto-grants-2010_06 |
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| ORD ID | ord-5f9779b5c3244eb2a6fd38a7490201d2 |
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| 出典メモ | uspto-grants-2010_06 |
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