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Acetic Acid → Ethyl 3-(5-(2-(((4-bromo-2-fluorophenyl)amino)methyl)-5-chlorophenyl)picolinamido)propanoate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Acetic Acid | HCID 176 | — |
| 反応物 | 4-Bromo-2-fluoroaniline | HCID 123050 | — |
| 反応物 | Sodium triacetoxyborohydride | HCID 5049666 | — |
| 反応物 | Ethyl 3-(5-(5-chloro-2-formylphenyl)picolinamido)propanoate | HCID 86674246 | — |
| 溶媒 | 1,2-Dichloroethane | HCID 11 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | Ethyl 3-(5-(2-(((4-bromo-2-fluorophenyl)amino)methyl)-5-chlorophenyl)picolinamido)propanoate | HCID 71059944 | — |
反応手順
Solid NaBH(OAc)3 (623 mg, 2.9 mmol) was added to a DCE solution (3 mL) of ethyl 3-(5-(5-chloro-2-formylphenyl)picolinamido)propanoate, prepared as describe in Example 6, (530 mg, 1.5 mmol), 4-bromo-2-fluoroaniline (293 g, 1.5 mmol), and AcOH (0.34 mL, 5.9 mmol) and the resulting mixture was stirred at room temperature. After 16 h the resulting mixture diluted with EtOAc washed with water and brine, dried (Na2SO4), dry-packed onto silica gel and purified via column chromatography to yield 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-8c2df863289d440eaae1917cecead34c |
| 出典メモ | uspto-grants-2014_06 |