関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Formic Acid | HCID 284 | — |
| 反応物 | Acetic Anhydride | HCID 7918 | — |
| 反応物 | 2-Chloro-3-fluoroaniline | HCID 88884 | — |
| 生成物 | N-(2-Chloro-3-fluorophenyl)formamide | HCID 57346568 | 95.1% |
反応手順
A solution of acetic anhydride (10 mL, 106 mmol) and formic acid (30 mL, 795 mmol) was stirred at room temperature for 10 mins. 2-Chloro-3-fluoroaniline (2.9 g, 20 mmol) was added and the reaction mixture was stirred at 60° C. for 1.5 h. After cooling to room temperature, the solvents were removed in vacuo and the residue was redissolved in DCM (100 mL) and was washed with sat aq. NaHCO3 until the aqueous phase had a measured pH of 8. The organic layer was further washed with water (2×100 mL), separated and dried over MgSO4. Filtration and concentration in vacuo gave N-(2-chloro-3-fluoro-phenyl)-formamide (3.3 g, 95%) as a colorless solid which did not require further purification. MS (M+H)+: 173.9, tR=2.04 min (method 1).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08481738B2 |
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| 出典データセット | uspto-grants-2013_07 |
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| ORD ID | ord-807a0f3beb274a029b1abffe55b10786 |
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| 出典メモ | uspto-grants-2013_07 |
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