Ammonium Chloride → 1,4-Dichlorophthalazin-6-amine
反応式
[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]=1参加物
5
実験手順
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.
後処理
- temperaturewas heated
- temperatureto reflux for 4 h
- concentrationthen concentrated
- washwashed with saturated aqueous NaHCO3, brine
- dry with materialdried (Na2SO4)
- concentrationconcentrated
出典と根拠
- ORDレコード
- ord-c23203620f4d42979d64eb9b6f98684e
- 出典データセット
- uspto-grants-2013_01
- 特許番号
- US08349836B2
反応ノート
読み込み中…