Hydrazine → 5-Tert-butyl-1H-pyrazolo[3,4-d]pyridazin-4(5H)-one
反応式
[C:1]([N:5]1[C:10](=[O:11])[C:9]([CH:12]=O)=[C:8]([N:14](C)C)[CH:7]=[N:6]1)([CH3:4])([CH3:3])[CH3:2].[NH2:17]N>C(O)C>[C:1]([N:5]1[C:10](=[O:11])[C:9]2[CH:12]=[N:17][NH:14][C:8]=2[CH:7]=[N:6]1)([CH3:4])([CH3:3])[CH3:2]参加物
4
実験手順
2-Tert-butyl-5-dimethylamino-4-formyl-3(2H)-pyridazinone (3.5 g) was added to hydrazine (5.1 g)/ethanol (30 ml) and the mixture was refluxed for 40 hours. The solvent ethanol-hydrazine was then distilled off and the residue was extracted with ethyl acetate. The organic layer was washed with saturated aqueous NaCl solution, dried over anhydrous magnesium sulfate, and concentrated to dryness. The residue was washed with n-hexane-diethyl ether and dried. White powder, 1.9 g. 1H-NMR (CDCl3) δ: 1.71(9H,s), 8.19(1H,s), 8.32(1H,s).
後処理
- temperaturethe mixture was refluxed for 40 hours
- distillationThe solvent ethanol-hydrazine was then distilled off
- extractionthe residue was extracted with ethyl acetate
- washThe organic layer was washed with saturated aqueous NaCl solution
- dry with materialdried over anhydrous magnesium sulfate
- concentrationconcentrated to dryness
- washThe residue was washed with n-hexane-diethyl ether
- customdried
出典と根拠
- ORDレコード
- ord-585dbe4cf4c84746b9db287b5f2cf064
- 出典データセット
- uspto-grants-1998_05
- 特許番号
- US05753664
反応ノート
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