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Sodium borohydride → N-(6-chloropyridin-3-yl)-2-aminobenzamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Sodium borohydride | HCID 4311764 | — |
| 反応物 | N-(6-chloropyridin-3-yl)-2-nitrobenzamide | HCID 21906170 | — |
| 触媒 | Nickel acetate tetrahydrate | HCID 62601 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | N-(6-chloropyridin-3-yl)-2-aminobenzamide | HCID 21906549 | 46% |
反応手順
To a stirred solution of N-(6-chloropyridin-3-yl)-2-nitrobenzamide (0.6 g, 2.15 mmol) in methanol (150 mL) and tetrahydrofuran (75 mL) was added nickel acetate tetrahydrate (1.07 g, 4.3 mmol). Sodium borohydride (0.326 g, 8.61 mmol) was then added in small portions. After gas evolution had ceased, the solvent was removed in vacuo. The residue was partitioned between ethyl acetate and concentrated ammonium hydroxide, and the layers separated. The organic phase was washed with concentrated ammonium hydroxide and saturated aqueous sodium chloride solution, dried (magnesium sulfate), filtered, and concentrated in vacuo. The solid was suspended in ether, sonicated, and filtered to give 0.243 g (46%) of a pink solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07129245B2 |
| 出典データセット | uspto-grants-2006_10 |
| ORD ID | ord-4a5526ea2a04459ab92705179946e3b2 |
| 出典メモ | uspto-grants-2006_10 |