関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Dimethylformamide | HCID 6228 | — |
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | 2-(Nitromethylene)imidazolidine | HCID 3014763 | — |
| 反応物 | 3-Methoxy-2-nitro-6-pyridylmethyl bromide | HCID 14405124 | — |
| 反応物 | HCID 178418361 | HCID 178418361 | — |
| 生成物 | 1-(3-Methoxy-2-nitro-6-methylpyridylmethyl)-2-nitromethyleneimidazolidine | HCID 86742440 | — |
反応手順
Nitromethyleneimidazolidine (1.3 g) was dissolved in dry dimethylformamide (15 ml), and sodium hydride (0.26 g) was added. The mixture was stirred at room temperature until the generation of hydrogen ceased. Subsequently, a solution of 2.4 g of 3-methoxy-2-nitro-6-pyridylmethyl bromide in 5 ml of dimethylformamide was added, and the mixture was stirred at 60° C. for 15 minutes. The reaction mixture was cooled to room temperature, poured into 50 ml of ice water, and extracted with dichloromethane. Dichloromethane was distilled off under reduced pressure, and ethanol was added to the residue to precipitate crystals. The crystals were collected by filtration and washed with ethanol to give 1-(3-methoxy-2-nitro-6-methylpyridylmethyl)-2-nitromethyleneimidazolidine (0.4 g). mp. 177°-181° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04772620 |
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| 出典データセット | uspto-grants-1988_09 |
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| ORD ID | ord-4cdc866464844c1c9043c9b082818713 |
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| 出典メモ | uspto-grants-1988_09 |
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