Sulfuric Acid → 2,3-Dichloro-5-methyl-1H-pyrrolo[2,3-d]pyridazin-4(5H)-one
反応式
[CH3:1][NH:2][NH2:3].[C:4]([C:9]1[C:13]([Cl:14])=[C:12]([Cl:15])[NH:11][C:10]=1[CH:16]=O)(OCC)=[O:5].S(=O)(=O)(O)O>C(O)C>[Cl:15][C:12]1[NH:11][C:10]2[CH:16]=[N:3][N:2]([CH3:1])[C:4](=[O:5])[C:9]=2[C:13]=1[Cl:14]参加物
5
実験手順
A solution of methylhydrazine (4.72 g) and 3-carbethoxy-4,5-dichloro-2-formylpyrrole (4.72 g) in ethanol (50 ml) was refluxed for 2 hours. After cooling to room temperature, concentrated sulfuric acid (0.5 ml) was added and the mixture was refluxed for another 21 hours. The reaction mixture was cooled to room temperature and the resulting crystals were collected by filtration. The crystals were rinsed with ethanol and ether and dried in vacuo to provide the title compound as brown powder (3.29 g; yield 81%). H-NMR (DMSO-d6) δ: 3.66(3H,s), 8.11(1H,s).
後処理
- temperaturethe mixture was refluxed for another 21 hours
- temperatureThe reaction mixture was cooled to room temperature
- filtrationthe resulting crystals were collected by filtration
- washThe crystals were rinsed with ethanol and ether
- customdried in vacuo
出典と根拠
- ORDレコード
- ord-9896931c0ddc4db5be803d3e9cca8f8d
- 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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