関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Cesium carbonate | HCID 10796 | — |
| 反応物 | Binap, (A+-)- | HCID 634876 | — |
| 反応物 | 5,6-Dimethoxypyridin-2-amine | HCID 46739148 | — |
| 反応物 | Methyl 4-(8-bromoimidazo[1,2-b]pyridazin-6-yl)benzoate | HCID 86682706 | — |
| 触媒 | Bis(dibenzylideneacetone)palladium | HCID 9811564 | — |
| 溶媒 | 1,4-Dioxane | HCID 31275 | — |
| 生成物 | Methyl 4-(8-(5,6-dimethoxypyridin-2-ylamino)imidazo[1,2-b]pyridazin-6-yl)benzoate | HCID 86682718 | 141.3% |
反応手順
A mixture of methyl 4-(8-bromoimidazo[1,2-b]pyridazin-6-yl)benzoate (0.3 g, 0.904 mmol), 5,6-dimethoxypyridin-2-amine (0.167 g, 1.084 mmol), Pd2(dba)3 (52 mg, 0.09 mmol), BINAP (225 mg, 0.362 mmol) and Cs2CO3 (0.884 g, 2.712 mmol) in dioxane (20 mL) was heated to 100° C. for 16 h in a sealed tube under N2 atmosphere. The mixture was cooled and concentrated in vacuo. The residue was purified by chromatography (silica, 10 g, 200-300 mesh, ethyl acetate:petroleum ether=1:3) to afford methyl 4-(8-(5,6-dimethoxypyridin-2-ylamino)imidazo[1,2-b]pyridazin-6-yl)benzoate (0.518 g) as a yellow solid containing unidentified impurities. LC-MS: [M+H]+=406, tR=1.766 min.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US09169259B2 |
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| 出典データセット | uspto-grants-2015_10 |
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| ORD ID | ord-ca69b1522e704a6299a0b834f98f415d |
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| 出典メモ | uspto-grants-2015_10 |
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