化工社化工社 化学情報印刷レポート · 研究参考用
Hydrochloric Acid → (3-Bromopyridin-2-yl)methanamine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Sodium Chloride | HCID 5234 | — |
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | 3-Bromopyridine-2-carbonitrile | HCID 817694 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | (3-Bromopyridin-2-yl)methanamine | HCID 46398142 | — |
反応手順
3-Bromo-pyridin-2-nitrile (14.3 g, 78.0 mmol) was dissolved in 200 mL of dry THF. While stirring the solution, 100 mL of BH3-THF complex (1M) (5 eq) was added drop-wise. The mixture was then stirred overnight and 250 mL 4N HCl were added and the solution was refluxed for additionally 30 min. After that a 2M aqueous solution of NaOH (pH-value=8.0). The mixture was saturated by addition of NaCl. The organic layer was separated and the aqueous solution was again extracted three times by means of 100 mL THF. The organic layers were combined and dried over Na2SO4. After that the solvent was removed and the remaining oil was used without further purification.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07803810B2 |
| 出典データセット | uspto-grants-2010_09 |
| ORD ID | ord-e722bfb383644a139d6d9878c3d942ce |
| 出典メモ | uspto-grants-2010_09 |