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

HRID 1417746노트

반응식

HRID 1417746 반응식
[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

참가 물질

5

반응물 3

HCID 8028TetrahydrofuranHCID 121435644-Chloro-2-iodo-6-nitroanilineHCID 178418361HCID 178418361, 화합물

생성물 1

HCID 540159985-Chloro-3-iodobenzene-1,2-diamine수율 96.3%

시약·촉매·용매 1

HCID 10311-Propanol용매

실험 절차

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.

후처리

  1. customis carried out at 130° C.
  2. filtrationthe catalyst is filtered off
  3. filtrationAfter filtration
  4. customthe solvent is removed by distillation

출처 및 근거

ORD 기록
ord-a96c476860a947fe84554ab6a145ed73
출처 데이터셋
uspto-grants-1999_03
특허 번호
US05877340

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