Sulfuric Acid → 2,3-Dichloro-5-methyl-1H-pyrrolo[2,3-d]pyridazin-4(5H)-one
반응식
[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]참가 물질
5
실험 절차
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).
후처리
- 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
출처 및 근거
- ORD 기록
- ord-9896931c0ddc4db5be803d3e9cca8f8d
- 출처 데이터셋
- uspto-grants-1998_05
- 특허 번호
- US05753664
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