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Nitric Acid → 3-Nitrophenylguanidine Nitrate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Nitric Acid | HCID 944 | — |
| 反応物 | 3-Nitroaniline | HCID 7423 | — |
| 反応物 | Cyanamide | HCID 9864 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | 3-Nitrophenylguanidine Nitrate | HCID 178512513 | 57% |
反応手順
A mixture of 3-nitroaniline (50 mmol, 6.90 g) in EtOH (10 mL) was cooled on an ice bath. Nitric acid (69% aq. soln.; 3.6 mL) was added dropwise. To this mixture cyanamide (50% aq soln.; 5 mL) was added. The reaction mixture was stirred at r.t. for 10 min and was then refluxed under N2 for a further 22 h. The solvent was evaporated. The dark brown solid was washed with EtOAc/EtOH and dried-under high vacuum overnight to afford the title compound as a brown solid (6.90 g, 57%). 1H-NMR (300 MHz, DMSO-d6) δ7.66-7.75 (m, 2H, Ph-H), 8.09-8.14 (m, 2H, Ph-H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06699854B2 |
| 出典データセット | uspto-grants-2004_03 |
| ORD ID | ord-22913f1654784eeab53d85fc59c0827c |
| 出典メモ | uspto-grants-2004_03 |