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HRID 226040作成日:2026年10月26日
Cesium carbonate → 8-(1-Ethyl-propyl)-3-(3,5-dimethyl-benzo[b]thiophen-2-yl)-2,6-dimethyl-imidazo[1,2-b]pyridazine
https://huagongshe.com/reaction/226040
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Cesium carbonate | HCID 10796 | — |
| 反応物 | Triphenylphosphine | HCID 11776 | — |
| 反応物 | 3-Methylbenzo[b]thiophene | HCID 73817 | — |
| 反応物 | 8-(1-Ethyl-propyl)-3-iodo-2,6-dimethyl-imidazo[1,2-b]pyridazine | HCID 57752681 | — |
| 触媒 | Bis(dibenzylideneacetone)palladium | HCID 9811564 | — |
| 溶媒 | Diethyl Ether | HCID 3283 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 8-(1-Ethyl-propyl)-3-(3,5-dimethyl-benzo[b]thiophen-2-yl)-2,6-dimethyl-imidazo[1,2-b]pyridazine | HCID 57752606 | 85% |
反応手順
A mixture of 8-(1-ethyl-propyl)-3-iodo-2,6-dimethyl-imidazo[1,2-b]pyridazine (0.145 mmol), 3-methyl-benzo[b]thiophene (7.25 mmol), Pd2 dba3 (0.0072 mmol), triphenylphosphine (0.029 mmol), and cesium carbonate (0.29 mmol) in previously degassed DMF (0.5 ml) is added to a pressure tube with a stirring bar. The mixture is degassed for 30 min. After heating for 16 h at 130° C., reaction mixture is cooled, diluted with diethylether and washed with saturated aqueous ammonium chloride solution. The organic layer is dried over anhydrous magnesium sulfate, filtered, and the solvent is removed in vacuo. The residue is purified by silica gel column chromatography using mixtures of hexane-ethyl acetate as eluent to give the title compound (85%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07557103B2 |
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| 出典データセット | uspto-grants-2009_07 |
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| ORD ID | ord-ae5b6238cd8747faba4bf0158a24b4f7 |
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| 出典メモ | uspto-grants-2009_07 |
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