Tetrahydrofuran → 5-Chloro-3-iodobenzene-1,2-diamine

HRID 1417746ノート

反応式

HRID 1417746 の反応式
[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

  1. customis carried out at 130° C.
  2. filtrationthe catalyst is filtered off
  3. filtrationAfter filtration
  4. 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

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