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Hydrochloric Acid → 2-Azido-6-chloropyridine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Diethyl Ether | HCID 3283 | — |
| 反応物 | 2-Chloro-6-hydrazinopyridine | HCID 320004 | — |
| 反応物 | Sodium Nitrite | HCID 23668193 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 2-Azido-6-chloropyridine | HCID 21576379 | — |
反応手順
To a 250 ml round-bottom flask equipped with a mechanical stirrer, a Claisen head and an addition funnel were added 2-chloro-6-hydrazinopyridine (4.00 g, 27.9 mmol), Et2O (20 mL) and concentrated hydrochloric acid (12 mL, 146 mmol). A solution of sodium nitrite (2.211 g, 32.0 mmol) in water (28 mL) was added dropwise to the cooled (0° C.) reaction mixture. The insoluble starting material gradually dissolved. After 2 h, the aqueous phase was extracted with ether (2×50 mL). The combined organic phase was dried over MgSO4, and concentrated in vacuo to provide the title compound as yellow crystals: LCMS m/z 155.14 [M+H]+.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08455638B2 |
| 出典データセット | uspto-grants-2013_06 |
| ORD ID | ord-1f009bfbd0c34d87ad55aef5e540ebe1 |
| 出典メモ | uspto-grants-2013_06 |