関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Cesium carbonate | HCID 10796 | — |
| 反応物 | Iodobenzene | HCID 11575 | — |
| 反応物 | 5-Chloro-1,10-phenanthroline | HCID 77865 | — |
| 反応物 | HCID 47197229 | HCID 47197229 | — |
| 反応物 | Water ammonium hydroxide | HCID 86589665 | — |
| 溶媒 | N-methyl-2-pyrrolidone | HCID 13387 | — |
| 生成物 | HCID 87449702 | HCID 87449702 | — |
反応手順
To a 4 mL vial equipped with a septum cap and stir bar was added N-(5-methyl-1,3-thiazol-2-yl)pyrrolidine-1-carboxamide (21 mg, 0.1 mmol), copper(I) trifluoromethanesulfonate benzene complex (10 mg, 0.02 mmol), 5-chloro-1,10-phenanthroline (8.5 mg, 0.04 mmol) and cesium carbonate (38.9 mg, 0.12 mmol). The mixture was placed under a nitrogen atmosphere. Iodobenzene (0.12 mmol) in 1-methyl-2-pyrrolidinone (1.0 mL) was added to the mixture. The reaction mixture was heated at 120° C. for overnight. A solution of concentrated ammonium hydroxide/water (1:2, 1 mL) was added and the mixture was filtered and solvent removed under reduced pressure. The residue was purified by reverse phase HPLC (C8, gradient 10-100% acetonitrile/water/0.1% trifluoroacetic acid).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08383657B2 |
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| 出典データセット | uspto-grants-2013_02 |
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| ORD ID | ord-b9a1c7ad96754a8e8302465963d697d4 |
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| 出典メモ | uspto-grants-2013_02 |
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