Ammonium Chloride → 1,4-Dichlorophthalazin-6-amine
반응식
[Cl:1][C:2]1[C:11]2[C:6](=[CH:7][C:8]([N+:12]([O-])=O)=[CH:9][CH:10]=2)[C:5]([Cl:15])=[N:4][N:3]=1.[NH4+].[Cl-]>[Fe].CCO>[Cl:1][C:2]1[C:11]2[C:6](=[CH:7][C:8]([NH2:12])=[CH:9][CH:10]=2)[C:5]([Cl:15])=[N:4][N:3]=1참가 물질
5
실험 절차
A mixture of 1,4-dichloro-6-nitro-phthalazine (1.24 g, 5.09 mmol), EtOH (20 mL), saturated aqueous NH4Cl (20 mL) and iron powder (1.42 g, 25.47 mmol) was heated to reflux for 4 h then concentrated. The residue was taken up in EtOAc washed with saturated aqueous NaHCO3, brine, dried (Na2SO4) and concentrated. Column chromatography (Hexanes/EtOAc) afforded the desired product (0.33 g, 30%) as a pale yellow solid.
후처리
- temperaturewas heated
- temperatureto reflux for 4 h
- concentrationthen concentrated
- washwashed with saturated aqueous NaHCO3, brine
- dry with materialdried (Na2SO4)
- concentrationconcentrated
출처 및 근거
- ORD 기록
- ord-f6423bb330234ae291f289a4878fada7
- 출처 데이터셋
- uspto-grants-2011_10
- 특허 번호
- US08044041B2
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