Tetrahydrofuran → 5-Chloro-3-iodobenzene-1,2-diamine
反応式
[Cl:1][C:2]1[CH:8]=[C:7]([N+:9]([O-])=O)[C:5]([NH2:6])=[C:4]([I:12])[CH:3]=1.O1CCCC1.[H][H]>C(O)CC>[Cl:1][C:2]1[CH:3]=[C:4]([I:12])[C:5]([NH2:6])=[C:7]([NH2:9])[CH:8]=1参加物
5
実験手順
1.5 g of 4-chloro-2-iodo-6-nitroaniline together with 50 ml of tetrahydrofuran and 10 ml of 1-propanol are initially introduced into a stirred autoclave. 5 mg of FeCl2.4H2O and 0.3 g Pt/Pb-CaCO3 catalyst are added to the solution, and hydrogenation is carried out at 130° C. and 20 bar of hydrogen. After the hydrogenation has come to a standstill, the reaction mixture is cooled to room temperature, the reactor is rendered inert with nitrogen and the catalyst is filtered off. After filtration, the solvent is removed by distillation to give 1.3 g of 4-chloro-6-iodo-1,2-phenylenediamine as a crude product.
後処理
- customis carried out at 130° C.
- filtrationthe catalyst is filtered off
- filtrationAfter filtration
- customthe solvent is removed by distillation
出典と根拠
- ORDレコード
- ord-a96c476860a947fe84554ab6a145ed73
- 出典データセット
- uspto-grants-1999_03
- 特許番号
- US05877340
反応ノート
読み込み中…