関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Nitrogen | HCID 947 | — |
| 反応物 | L-Canaline | HCID 441443 | — |
| 反応物 | Methyl hydrazinecarbimidothioate hydroiodide | HCID 6508896 | — |
| 溶媒 | Sodium Hydroxide | HCID 14798 | — |
| 生成物 | 2-Amino-4-[2-(hydrazinoimino-methyl)hydrazino]-butanoic acid | HCID 54036615 | — |
反応手順
Mix canaline (2.65 g, 20 mmol) and S-methylisothiosemicarbazide hydroiodide (4.66 g, 20 mmol) in 1M NaOH (40 ml) and stir under a blanket N2 at 40° C. for 48 hours. Neutralize the reaction with 1M HCl and blow to a residue with a stream of N2. Apply the residue to a Dowex AG50-X8 column and elute with 0.2M NH4OH. Lyophilize the fractions containing the desired product and take up the resulting solid in water (20 ml). Add flavianic acid (3.2 g) in water (20 ml) and cool the solution to 4° C. for 16 hours. Filter the resulting solid and crystallize to yield the title compound.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US05318992 |
|---|
| 出典データセット | uspto-grants-1994_06 |
|---|
| ORD ID | ord-c8cda447d7c7482da4b25906b25fe5f4 |
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| 出典メモ | uspto-grants-1994_06 |
|---|
