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Acetonitrile → 1-Ethyl-N-methyl-N-pyridin-2-yl-1H-benzimidazol-2-amine
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 | Pivaloyl chloride | HCID 62493 | — |
| 反応物 | Bis(2-pyridylmethyl)amine | HCID 73759 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 1-Ethyl-N-methyl-N-pyridin-2-yl-1H-benzimidazol-2-amine | HCID 66628267 | — |
反応手順
To a flask were added 1.06 g of di-(2-picolyl)amine and 20 ml of acetonitrile. The solution was stirred under nitrogen, when 0.7 g of triethylamine were added, followed by 1.5 g of trimethylacetyl chloride. After 1 hour, 20 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 recrystallized by dissolving in 6 ml hot hexane with 0.5 ml 2-propanol. Another 2 ml hexane were added and the mixture was cooled to 5 C, filtered, washed with hexane and dried, resulting in 1.3 g of an off-white solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07525717B2 |
| 出典データセット | uspto-grants-2009_04 |
| ORD ID | ord-77e8045bcfe8450a9977152da9d76c2c |
| 出典メモ | uspto-grants-2009_04 |