関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 3-Methyl-4-(methylthio)phenol | HCID 18391 | — |
| 反応物 | 2-(Chloromethyl)-1-methyl-5-nitro-1H-imidazole | HCID 13032133 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 1-Methyl-2-(3-methyl-4-methylthiophenyloxymethyl)-5-nitro-imidazole | HCID 54473381 | — |
反応手順
To a solution of 15.4 g (0.1 mol) of 3-methyl-4-methylmercaptophenol in 30 ml of dimethylformamide, 13.8 g (0.1 mol) of potassium carbonate powder are added, and then a solution of 17.6 g (0.1 mol) of 1-methyl-2-chloromethyl-5-nitro-imidazole in 40 ml of dimethylformamide is added dropwise while stirring at 25° C. The temperature of the faintly exothermal reaction is adjusted to at most 35° C. by cooling with ice water. The mixture is then stirred for another hour at 25° C., poured onto ice/water, the precipitate is suction-filtered, washed with water and recrystallized from methanol with an addition of charcoal to yield 21.7 g (74% of the theoretical yield) of 1-methyl-2-(3-methyl-4-methylthiophenyl-oxymethyl)-5-nitro-imidazole in the form of yellow crystals, m.p. 108° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04042705 |
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| 出典データセット | uspto-grants-1977_08 |
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| ORD ID | ord-7a0a46fecb9046b0b4951a4a38cda529 |
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| 出典メモ | uspto-grants-1977_08 |
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