関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 5-(Tributylstannyl)pyrimidine | HCID 2763249 | — |
| 反応物 | 2-Dicyclohexylphosphino-2',4',6'-triisoprophylbiphenyl | HCID 11155794 | — |
| 反応物 | 2-Bromo-7-methoxy-9H-xanthen-9-one | HCID 57475633 | — |
| 触媒 | Bis(dibenzylideneacetone)palladium | HCID 9811564 | — |
| 溶媒 | 1,4-Dioxane | HCID 31275 | — |
| 生成物 | 2-methoxy-7-(pyrimidin-5-yl)-9H-xanthen-9-one | HCID 57475654 | 60.2% |
反応手順
A vial charged with Pd2(dba)3 (0.150 g, 0.164 mmol), XPhos (0.391 g, 0.819 mmol), 5-(tributylstannyl)pyrimidine (1.81 g, 4.92 mmol), 2-bromo-7-methoxy-9H-xanthen-9-one (1.000 g, 3.28 mmol) and dioxane (10 mL). The reaction mixture was evacuated and backfilled with nitrogen. The reaction mixture was heated to 100° C. overnight. The reaction mixture was cooled to RT and diluted with water and EtOAc. A grey solid precipitated out, which was filtered off. The solid was washed with EtOAc and water. The grey solid dried under reduced pressure to afford 2-methoxy-7-(pyrimidin-5-yl)-9H-xanthen-9-one) (0.600 g, 60.2% yield).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US08497264B2 |
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| 出典データセット | uspto-grants-2013_07 |
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| ORD ID | ord-7e96cc4aacfa414a9927a9d5c3bd74cc |
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| 出典メモ | uspto-grants-2013_07 |
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