関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Ethyl isocyanate | HCID 8022 | — |
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | 2-Aminobenzothiazole-6-carbonitrile | HCID 4327139 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | N-(6-Cyano-1,3-benzothiazol-2-yl)-N'-ethylurea | HCID 21985533 | — |
反応手順
2-Amino-1,3-benzothiazole-6-carbonitrile (0.2 g) was dissolved in about 5 mL dimethylformamide. About 0.2 mL of ethylisocyanate was added, followed by about 0.3 mL triethylamine and the solution was heated to about 80° C. under good agitation. The solution was allowed to stir for about 4 hours then cooled to room temperature. The solvent was removed in vacuo and the solids were washed well with ether. The product was further purified by column chromatography and after drying in vacuo, about 0.14 grams was isolated. 1H NMR 1.1 (t, 3H, J=7.2 Hz), 3.2 (m, 2H), 6.8 (s, 1H), 7.7 (m, 2H), 8.4 (s, 1H), 11.0 (s, 1H), LC/MS 2.54 min, 247 (MH+), 245 (M−H−), lab RP-HPLC RT 7.8 minutes.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07091227B2 |
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| 出典データセット | uspto-grants-2006_08 |
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| ORD ID | ord-4bb201544c5043cd978fe2b16f5062ab |
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| 出典メモ | uspto-grants-2006_08 |
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