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Hydrazine hydrate (1:1) → 4-(3,4-Dimethoxy-phenyl)-4a,5,8,8a-tetrahydro-2H-phthalazin-1-one
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 | 6-(3,4-Dimethoxy-benzoyl)-cyclohex-3-enecarboxylic acid | HCID 22219622 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | 4-(3,4-Dimethoxy-phenyl)-4a,5,8,8a-tetrahydro-2H-phthalazin-1-one | HCID 22337182 | — |
反応手順
A mixture of 6-(3,4-dimethoxy-benzoyl)-cyclohex-3-enecarboxylic acid (112 mg, 0.39 mmol, 1.0 eq) and hydrazine hydrate (31 mg, 0.96 mmol, 2.5 eq) in EtOH (3 mL) was refluxed for 4 hr. The reaction was then cooled to room temperature and then concentrated under reduced pressure to oil. The oil was dissolved in EtOAc and washed with water followed by brine. The organic layer was then dried over Na2SO4, filtered through paper, and concentrated under reduced pressure to oil. The product was recrystallized in EtOH to yield a white solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08168635B2 |
| 出典データセット | uspto-grants-2012_05 |
| ORD ID | ord-899a43dff08b4dcb9e20254a2ca96e05 |
| 出典メモ | uspto-grants-2012_05 |