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Ammonium Hydroxide → 5-(Aminomethyl)pyridin-2-amine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Ammonium Hydroxide | HCID 14923 | — |
| 反応物 | 2-Amino-5-cyanopyridine | HCID 818260 | — |
| 反応物 | Borane;tetrahydrofuran | HCID 2723981 | — |
| 溶媒 | Hydrochloric Acid | HCID 313 | — |
| 生成物 | 5-(Aminomethyl)pyridin-2-amine | HCID 15766771 | 83.1% |
反応手順
To a solution of 6-aminonicotinonitrile 117-A (5.0 g, 42 mmol) was added a solution of 1 M BH3-THF (294 mL, 294 mmol) at 0° C. (prepared as in J.Org. Chem., Vol. 38, No. 5, 1973). The reaction was stirred at room temperature for 1 hour. The reaction mixture was then slowly pored into ice water. 100 mL 4N HCl was added and stirred for 20 min. The solution was basified with NH4OH to pH of about 11, and then concentrated. THF (300mL×2) was added to the mixture followed by addition of solid KOH (excess). The suspension was stirred. The THF layer was collected by filtration and concentrated to give 5-(aminomethyl)pyridin-2-amine 117-B (4.3 g).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07381824B2 |
| 出典データセット | uspto-grants-2008_06 |
| ORD ID | ord-dc84e24aea9d480893515ad0ec3b381a |
| 出典メモ | uspto-grants-2008_06 |