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Hydrochloric Acid → 1-Methyl-2-nitro-1H-imidazole-5-methanol
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Ethyl 1-methyl-2-nitro-1H-imidazole-5-carboxylate | HCID 329608 | — |
| 反応物 | Lithium borohydride | HCID 4148881 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 1-Methyl-2-nitro-1H-imidazole-5-methanol | HCID 70292 | 33% |
反応手順
To 0.2 g. of 5-carbethoxy-1-methyl-2-nitroimidazole in 30 ml. of tetrahydrofuran, 0.044 g. of LiBH4 is gradually added under stirring at room temperature. After stirring for 48 hours, the excess of LiBH4 is decomposed with 10% hydrochloric acid, the reaction mixture is filtered and the filtrated is evaporated to dryness under vacuum. The residue is taken up with acetone. Inorganic salts are filtered off and the solution is evaporated. The oily residue is chromatographed through 7 g. of silica gel, by eluting with chloroform containing from 1% to 3% (v/v) of methanol. After concentration of the portions containing the product, 0.052 g. (33%) of 1-methyl-2-nitro-5-hydroxymethylimidazole is obtained.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US03987053 |
| 出典データセット | uspto-grants-1976_10 |
| ORD ID | ord-a03961ce93cd4780a4d7fa4d01184531 |
| 出典メモ | uspto-grants-1976_10 |