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Hydrazine hydrate (1:1) → 3-(1,3-benzodioxol-5-yl)-N-[4-(hydrazinocarbonyl)phenyl]propanamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrazine hydrate (1:1) | HCID 24654 | — |
| 反応物 | Methyl 4-{[3-(1,3-benzodioxol-5-yl)propanoyl]amino}benzoate | HCID 9945244 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | 3-(1,3-benzodioxol-5-yl)-N-[4-(hydrazinocarbonyl)phenyl]propanamide | HCID 9858574 | 65% |
反応手順
To a suspension of methyl 4-{[3-(1,3-benzodioxol-5-yl)propanoyl]amino}benzoate (200 mg, 0.61 mmol) in EtOH (3.5 mL) was added hydrazine hydrate (0.5 mL). After stirring for 15 hrs at reflux, the reaction mixture was cooled to rt and a white solid precipitated out. Filtration, washing with EtOH (2×1 mL) and water (3×1 mL), and drying under vacuo at 70° C. for 1 hr gave 130 mg of the title compound (65%) as a white solid in 95.5% purity by HPLC (MaxPlot detection between 230 and 400 nm).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07696231B2 |
| 出典データセット | uspto-grants-2010_04 |
| ORD ID | ord-e8a46c128be04c3c98cd2040863afa19 |
| 出典メモ | uspto-grants-2010_04 |