関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Potassium Phosphate, Tribasic | HCID 62657 | — |
| 反応物 | 2-Amino-N-methylbenzamide | HCID 308072 | — |
| 反応物 | Bis[2-(diphenylphosphino)phenyl] ether | HCID 4285986 | — |
| 反応物 | 2,5-Dichloro-4-iodopyridine | HCID 53400965 | — |
| 触媒 | palladium(II) acetate | HCID 167845 | — |
| 溶媒 | 1,4-Dioxane | HCID 31275 | — |
| 生成物 | 2-[(2,5-Dichloro-4-pyridinyl)amino]-N-methylbenzamide | HCID 57516891 | 56.5% |
反応手順
A 150-mL sealed tube was charged with 2,5-dichloro-4-iodopyridine (3.5 g, 12.78 mmol), 2-amino-N-methylbenzamide (1.919 g, 12.78 mmol) and tripotassium phosphate (8.14 g, 38.3 mmol) in 1,4-dioxane (100 mL). The reaction mixture was degassed with nitrogen for 10 min. Bis(2-diphenylphosphinophenyl)ether (DPEPhos, 0.688 g, 1.278 mmol) and Pd(OAc)2 (0.115 g, 0.511 mmol) were added and the reaction mixture was heated in a 120° C. oil bath over night. The reaction mixture was filtered through celite, which was washed with dioxane. The solvent was evaporated to dryness and the solid was washed with EtOH (10 mL×3) to give 2.14 g (56%) of product as an off white solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US09446034B2 |
|---|
| 出典データセット | uspto-grants-2016_09 |
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| ORD ID | ord-63006ffb9bab4ecca372336ff57f1a83 |
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| 出典メモ | uspto-grants-2016_09 |
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