関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | 1-(6-Amino-1,3-benzodioxol-5-yl)ethan-1-one | HCID 120000 | — |
| 反応物 | 1-Benzofuran-3-carbonyl chloride | HCID 13024720 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | N-(6-acetyl-1,3-benzodioxol-5-yl)-1-benzofuran-3-carboxamide | HCID 44220313 | — |
反応手順
Into solutions of 154 (5.0 mmol) in 200 mL of dry toluene were added triethylamine (4 mL) and 2-amino-4,5-methylenedioxy acetophenone (148) (5 mmol). The mixtures were stirred at 20±2° C. for 24 h and then evaporated. The residues were washed with acetone and EtOH and then recrystallized from acetone or EtOH to form 155. Obtained as a pale-yellow solid; mp 144-145° C.; ESI-MS (Positive mode): m/z 324 [M+H]+; 1H-NMR (400 MHz, DMSO-d6): δ 2.63 (3H, s), 6.19 (2H, s), 7.41-7.50 (21-1, m), 7.68 (1H, s), 7.75 (1H, dd, J=1.6, 6.8 Hz), 8.15 (1H, dd, J=2.0, 8.8 Hz), 8.27 (1H, s), 8.71 (1H, s), 12.63 (1H, s); IR (KBr): 1635, 1677 (C═O) cm−1.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08524740B2 |
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| 出典データセット | uspto-grants-2013_09 |
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| ORD ID | ord-f9b04acd88cd445f8767056ebf37512a |
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| 出典メモ | uspto-grants-2013_09 |
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