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Sodium borohydride → [4-(Aminomethyl)phenyl]-n-{2-[n-(5-chloro(2-pyridyl))carbamoyl]phenyl}carboxamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Sodium borohydride | HCID 4311764 | — |
| 反応物 | n-{2-[n-(5-Chloro(2-pyridyl))carbamoyl]phenyl}(4-cyanophenyl)carboxamide | HCID 22596336 | — |
| 触媒 | Cobalt(II) chloride | HCID 24288 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | [4-(Aminomethyl)phenyl]-n-{2-[n-(5-chloro(2-pyridyl))carbamoyl]phenyl}carboxamide | HCID 18727608 | 32.3% |
反応手順
A mixture of N-{2-[N-(5-chloro(2-pyridyl))carbamoyl]phenyl}(4-cyanophenyl)carboxamide (1 g, 2.6 mmol, 1.0 equiv.), cobalt chloride (0.5 g, 3.85 mmol, 1.5 equiv.) and sodium borohydride (0.295 g, 7.8 mmol, 3.0 equiv.) in DMF (20 mL) was stirred at 0° C. to rt for 2.5 hr. The reaction was quenched with ice cubes, diluted with ethyl acetate (100 mL) and filtered through celite. The filtrate was washed with saturated aqueous NaHCO3. The organic layer was dried over MgSO4, filtered, evaporated and HPLC (C18 reversed phase) eluting with 0.1% TFA in H2O/CH3CN gave [4-(aminomethyl)phenyl]-N-{2-[N-(5-chloro(2-pyridyl))carbamoyl]phenyl}carboxamide (320 mg, 30%). MS found for C20H17ClN4O2 (M+H)+: 381.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07727982B2 |
| 出典データセット | uspto-grants-2010_06 |
| ORD ID | ord-25ac70975bee4da599786cc6820b43b6 |
| 出典メモ | uspto-grants-2010_06 |