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Formic Acid → 1-Methyl-5-nitroimidazole
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Formic Acid | HCID 284 | — |
| 反応物 | 4-Nitroimidazole | HCID 18208 | — |
| 溶媒 | Dimethyl Sulfate | HCID 6497 | — |
| 生成物 | 1-Methyl-5-nitroimidazole | HCID 18210 | 82% |
反応手順
202 parts of 5-nitroimidazole is dissolved in 600 parts of formic acid (90% by weight), 250 parts of dimethyl sulfate is added and the whole is heated for 6 hours. The formic acid is distilled off in vacuo. 420 parts of water is added to the residue, the whole cooled to from 0° to 5° C. and the unreacted 5-nitroimidazole (60 parts) is centrifuged off. The mixture is adjusted to pH 10 with aqueous ammonia solution (25% by weight) and the precipitate is separated at 0° to 5° C. 130 parts of 1-methyl-5-nitroimidazole having a melting point of 58° to 60° C. is obtained; this is equivalent to a yield of 82% of theory based on reacted 4(5)-nitroimidazole.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04021442 |
| 出典データセット | uspto-grants-1977_05 |
| ORD ID | ord-092cab30577549c3af8174dff40cb61c |
| 出典メモ | uspto-grants-1977_05 |