関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | 2-Methylpyridine | HCID 7975 | — |
| 反応物 | Dimethylacetamide | HCID 31374 | — |
| 反応物 | Butyllithium | HCID 178418339 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 溶媒 | Hexane | HCID 8058 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | 1-(Pyridin-2-yl)propan-2-one | HCID 95910 | — |
反応手順
2-Picoline (2 g) was dissolved in tetrahydrofuran (30 ml) and the solution was cooled to −75° C. Butyl lithium (14.73 ml. of a 1.6M-solution in hexane) was added dropwise and the mixture stirred for 2 h. Dimethylacetamide (1.87 ml) was then added dropwise and the reaction was allowed to warm up to room temperature and stirring was continued for a further 2 h. Water (8.6 ml) and 36% hydrochloric acid (1.3 ml) were added and after stirring for another 30 minutes, ethyl acetate was added. The separated solvent phase was washed with brine and then dried (MgSO4). On evaporation an oil was obtained and used without further purification.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US07358376B2 |
|---|
| 出典データセット | uspto-grants-2008_04 |
|---|
| ORD ID | ord-c860e9ab15ed44159a48e3e704908253 |
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| 出典メモ | uspto-grants-2008_04 |
|---|