関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | 1-Amino-4-methylpiperazine | HCID 81349 | — |
| 反応物 | 7-Nitro-1,4-benzodioxane-5-carbonyl chloride | HCID 20544745 | — |
| 溶媒 | Methyl Ethyl Ketone | HCID 6569 | — |
| 生成物 | N-(4-methyl-1-piperazinyl)-7-nitro-1,4-benzodioxane-5-carboxamide | HCID 20544699 | 55.8% |
反応手順
33 g of 1-amino-4-methylpiperazine were dissolved in 630 ml of methyl ethyl ketone. The mixture was cooled to 10° C. and 61 g of 7-nitro-1,4-benzodioxane-5-carbonyl chloride were introduced by portions. The mixture was stirred for two hours and then the solid was filtered off and washed with 150 ml of methyl ethyl ketone. The obtained product was purified by transformation into the base (M.P.: 212° C.) and recystallized by treatment with hydrochloric ethanol. 45 g of N-(4-methyl-1-piperazinyl)-7-nitro-1,4-benzodioxane-5-carboxamide were obtained (M.P.: 210° C. with one mole of water). The structure was confirmed by nuclear magnetic resonance and infrared analyses.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04255580 |
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| 出典データセット | uspto-grants-1981_03 |
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| ORD ID | ord-15a0016f5e2a4643903fc71c61d06e76 |
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| 出典メモ | uspto-grants-1981_03 |
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