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Cesium carbonate → 2-chloro-N-(2,4-dichloro-5-methoxyphenyl)-5-methylpyrimidin-4-amine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Cesium carbonate | HCID 10796 | — |
| 反応物 | 1,1'-(9,9-Dimethyl-9H-xanthene-4,5-diyl)bis(1,1-diphenylphosphine) | HCID 636044 | — |
| 反応物 | 2-Chloro-5-methylpyrimidin-4-amine | HCID 4302175 | — |
| 反応物 | 1-Bromo-2,4-dichloro-5-methoxybenzene | HCID 19607721 | — |
| 触媒 | Bis(dibenzylideneacetone)palladium | HCID 9811564 | — |
| 溶媒 | 1,4-Dioxane | HCID 31275 | — |
| 生成物 | 2-chloro-N-(2,4-dichloro-5-methoxyphenyl)-5-methylpyrimidin-4-amine | HCID 57516481 | — |
反応手順
To a solution of 2-chloro-5-methylpyrimidin-4-amine (44.8 mg, 0.31 mmol) in 1,4-dioxane (20 mL) was added 1-bromo-2,4-dichloro-5-methoxybenzene (96 mg, 0.37 mmol), Cs2CO3 (408 mg, 1.25 mmol), Pd2(dba)3 (37 mg, 0.04 mmol), and 4,5-bis(diphenylphosphino)-9,9-dimethyxanthene (Xant Phos, 70 mg, 0.12 mmol). The mixture was heated under reflux for 4 h under Ar. The solid was filtered off and the filtrate washed with brine (1×100 mL). The organic solution was separated and dried (Na2SO4). The solvent was removed in vacuo. The crude product was used for next reaction without purification.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07528143B2 |
| 出典データセット | uspto-grants-2009_05 |
| ORD ID | ord-ebd55804ccdd46bc9dd1df4e506352e1 |
| 出典メモ | uspto-grants-2009_05 |