참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Hydrochloric Acid | HCID 313 | — |
| 반응물 | Nitrogen | HCID 947 | — |
| 반응물 | L-Canaline | HCID 441443 | — |
| 반응물 | Methyl hydrazinecarbimidothioate hydroiodide | HCID 6508896 | — |
| 용매 | Sodium Hydroxide | HCID 14798 | — |
| 생성물 | 2-Amino-4-[2-(hydrazinoimino-methyl)hydrazino]-butanoic acid | HCID 54036615 | — |
반응 단계
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.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 특허 번호 | US05318992 |
|---|
| 출처 데이터셋 | uspto-grants-1994_06 |
|---|
| ORD ID | ord-c8cda447d7c7482da4b25906b25fe5f4 |
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| 출처 메모 | uspto-grants-1994_06 |
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