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2-Chloro-4,6-dimethyl-3-pyridinecarbonitrile → 4,6-Dimethylnicotinonitrile
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 2-Chloro-4,6-dimethyl-3-pyridinecarbonitrile | HCID 223261 | — |
| 反応物 | Tin atom | HCID 5352426 | — |
| 溶媒 | Hydrochloric Acid | HCID 313 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 4,6-Dimethylnicotinonitrile | HCID 243917 | 54% |
反応手順
23 g of 2-chloro-3-cyano-4,6-dimethylpyridine are dissolved in 185 ml of concentrated hydrochloric acid and 240 ml of water. 25.4 g of tin metal are added and the mixture is brought to 100° C. The reaction is monitored by thin layer chromatography (TLC). When the reaction is complete, the mixture is allowed to return to room temperature and filtered and the filtrate is neutralized using sodium hydroxide solution. The mixture is extracted with methylene chloride and the combined organic phases are washed with saturated aqueous sodium bicarbonate solution and dried over anhydrous magnesium sulphate. The solution is concentrated to give 5-cyano-2,4-dimethyl-pyridine in the form of a yellow precipitate.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05821255 |
| 出典データセット | uspto-grants-1998_10 |
| ORD ID | ord-51804f6f471e4dfb910e9c186bc95b92 |
| 出典メモ | uspto-grants-1998_10 |