関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Dimethylformamide | HCID 6228 | — |
| 反応物 | Diethyl cyanophosphonate | HCID 76257 | — |
| 反応物 | 4-(Trifluoromethyl)benzylamine | HCID 76804 | — |
| 反応物 | 5-Cyanomethyl-2-methoxybenzoic acid | HCID 17830574 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Triethylamine | HCID 8471 | — |
| 生成物 | 5-cyanomethyl-2-methoxy-N-(4-trifluoromethylbenzyl)benzamide | HCID 17830578 | — |
反応手順
To 2.55 g of publicly known 5-cyanomethyl-2-methoxybenzoic acid were added 50 ml of dimethylformamide, 2.57 g of 4-trifluoromethylbenzylamine, 2.66 g of diethyl cyanophosphonate and 2.00 ml of triethylamine, and the mixture was stirred for 20 minutes under cooling with ice and for 6 hours at room temperature. The reaction mixture was poured into water and extracted with ethyl acetate. After washed with water, then with saturated brine, the organic layer was dried over anhydrous sodium sulfate. Solvent was distilled off under reduced pressure, and the residue was crystallized from hexane-diethyl ether and collected by filtration to obtain 4.44 g of 5-cyanomethyl-2-methoxy-N-(4-trifluoromethylbenzyl)benzamide as colorless crystals. Melting point 124-125° C. Elemental analysis (%) C16H15F3N2O2 Calcd.(%) C, 62.07; H, 4.34; N, 8.04 Found (%) C, 62.03; H, 4.27; N, 7.99
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06706763B1 |
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| 出典データセット | uspto-grants-2004_03 |
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| ORD ID | ord-15fc2dc155604716b508d487d80a25d1 |
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| 出典メモ | uspto-grants-2004_03 |
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