関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Ethylenediamine | HCID 3301 | — |
| 反応物 | Ethanediimidoyl dichloride, dihydroxy- | HCID 135527345 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | HCID 176528397 | HCID 176528397 | — |
反応手順
Dichloroglyoxime (15.7 g, 0.10 mole) and methanol (400 ml) were placed in a one-liter, round-bottom flask. This solution was cooled to 5° C. by means of a salt-ice bath. While the solution was vigorously stirred, a solution of 12.0 g (0.20 mole) of ethylene diamine in 30 ml of methanol was added in one portion. The mixture was stirred for 10 minutes; then the solvent was removed at reduced pressure. The remaining solid was slurried with 20 ml of water and the crude 2,3-dioximinopiperazine was collected and washed with methanol. The crude product weighed 10.2 g (70%). It can be recrystallized from water (70% recovery) to give the pure compound, 2,3-dioximinopiperazine, with a melting point of 195°-196° C. (dec).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04539405 |
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| 出典データセット | uspto-grants-1985_09 |
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| ORD ID | ord-56f138788d8946b29ded30880144db62 |
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| 出典メモ | uspto-grants-1985_09 |
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