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Methane → 2-Chloro-6-methylpyridin-3-ol
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Methane | HCID 297 | — |
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | 2-Methyl-5-hydroxypyridine | HCID 14275 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | 2-Chloro-6-methylpyridin-3-ol | HCID 3015797 | 67.3% |
反応手順
5-Hydroxy-2-methylpyridine (1-014-01) (27.01 g) was dissolved in conc. hydrochloric acid (200 mL) and to the reaction mixture was bubbled chlorine gas at 68 to 74° C. After the reaction mixture was stood overnight, the volatile was removed by bubbling nitrogen gas. The reaction mixture was evaporated under reduced pressure to give the crystal residue. The crystal residue was dissolved in methanol, and treated with active charcoal. After recrystallization, the desired 2-chloro-3-hyroxy-6-methylpyridine (1-014-02) (23.96 g, 67.3%) was obtained.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08088924B2 |
| 出典データセット | uspto-grants-2012_01 |
| ORD ID | ord-604e928b5fc24605bec02905ecf4fae1 |
| 出典メモ | uspto-grants-2012_01 |