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Acetonitrile → 2,2-dimethyl-N,N-dipyridin-2-ylpropanamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Acetonitrile | HCID 6342 | — |
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | 2,2'-Dipyridylamine | HCID 14547 | — |
| 反応物 | Pivaloyl chloride | HCID 62493 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 2,2-dimethyl-N,N-dipyridin-2-ylpropanamide | HCID 66628090 | 60.3% |
反応手順
To a flask were added 2.0 g of 2,2′-dipyridylamine and 35 ml of acetonitrile. The solution was stirred under nitrogen and cooled to 5 C, when 1.5 g of triethylamine were added, followed by 1.5 g of trimethylacetyl chloride and the mixture was allowed to warm to 22 C. After 1 hour, 50 ml of water were added and the acetonitrile was removed. The product was extracted with ethyl acetate and washed with water. Following solvent removal, the product was purified by silica gel chromatography using 50% ethyl acetate in hexane, resulting in 1.8 g of an oil that solidified on standing.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07538931B2 |
| 出典データセット | uspto-grants-2009_05 |
| ORD ID | ord-d32b158d094b4ecfa6151c5f07d73876 |
| 出典メモ | uspto-grants-2009_05 |