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Water → Ethyl 3-(5-(2-formyl-5-(trifluoromethyl)phenyl)picolinamido)propanoate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 2-Bromo-4-(trifluoromethyl)benzaldehyde | HCID 3020373 | — |
| 反応物 | Ethyl 3-(5-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)picolinamido)propanoate | HCID 71059832 | — |
| 触媒 | Bis(cyclopenta-1,4-dien-1-yl(diphenyl)phosphane);dichloropalladium;iron(2+) | HCID 178418228 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 溶媒 | 1,4-Dioxane | HCID 31275 | — |
| 生成物 | Ethyl 3-(5-(2-formyl-5-(trifluoromethyl)phenyl)picolinamido)propanoate | HCID 86674249 | — |
反応手順
2-bromo-4-(trifluoromethyl)benzaldehyde (1.3 g, 5.1 mmol), ethyl 3-(5-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)picolinamido)propanoate, prepared as in example 19, (2.7 g, 7.7 mmol), Pd(dppf)Cl2 (421 mg, 0.5 mmol), and K2CO3 (1.4 g, 10.3 mmol) were dissolved in 1,4-dioxane (40 mL) and water (10 mL) and the resulting mixture was heated to 80° C. After 16 h the resulting mixture was cooled to room temperature, diluted with EtOAc, washed with water and brine, dried (Na2SO4), and dry packed onto silica gel. Column chromatography yielded the title compound.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08748624B2 |
| 出典データセット | uspto-grants-2014_06 |
| ORD ID | ord-f5cdc8a72be244d6966f94d960110110 |
| 出典メモ | uspto-grants-2014_06 |