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Diethyl Pyrocarbonate → Ethyl 5-butyryl-1,6-dimethyl-benzimidazole-2-carboxylate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Diethyl Pyrocarbonate | HCID 3051 | — |
| 反応物 | Acetonitrile | HCID 6342 | — |
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | 5-Butyryl-1,6-dimethyl-benzimidazole-2-carboxylic acid | HCID 12806665 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | Ethyl 5-butyryl-1,6-dimethyl-benzimidazole-2-carboxylate | HCID 12806645 | — |
反応手順
6.0 g of 5-butyryl-1,6-dimethyl-benzimidazole-2-carboxylic acid are introduced, in the course of 15 minutes, into a mixture of 150 ml of acetonitrile, 15 ml of triethylamine and 18.5 g of diethyl pyrocarbonate, while stirring at room temperature. The mixture is left to stand overnight, the acetonitrile is stripped off under reduced pressure, the residue is taken up in ethyl acetate and the resulting solution is washed with water, dried over sodium sulphate and evaporated to dryness. Ethyl 5-butyryl-1,6-dimethyl-benzimidazole-2-carboxylate, which is initially obtained as an oil but soon crystallises, is filtered off. When recrystallised from ethyl acetate/cyclohexane, it melts at 106°-108°.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04344957 |
| 出典データセット | uspto-grants-1982_08 |
| ORD ID | ord-f9bbc6572ec74a20b197f28a15b1a56a |
| 出典メモ | uspto-grants-1982_08 |