1-Chloro-2,4-Dinitrobenzene → 4-Chloro-M-phenylenediamine

HRID 1087988

반응식

HRID 1087988 반응식
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([N+:8]([O-])=O)=[CH:4][C:3]=1[N+:11]([O-])=O.C(O)(=O)C.C(N)=N.[H][H]>[Ni].CO>[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([NH2:8])=[CH:4][C:3]=1[NH2:11]

참가 물질

6

반응물 3

HCID 61-Chloro-2,4-DinitrobenzeneHCID 160693Formamidine acetateHCID 178418361HCID 178418361, 화합물

생성물 1

HCID 212094-Chloro-M-phenylenediamine

시약·촉매·용매 2

HCID 935Nickel촉매HCID 887Methanol용매

실험 절차

40.8 g of 1-chloro-2,4-dinitrobenzene, 2 g of Raney nickel (60%, aqueous), 1.5 g of formamidine acetate and 120 ml of methanol are introduced in an autoclave equipped with gas introduction stirrer. The air in the autoclave is then displaced by nitrogen and then by hydrogen. The hydrogenation is carried out at a pressure of 10 bar and a temperature of 60° C. The hydrogenation time is 11/4 hours. 1-Chloro-2,4-diaminobenzene, 99% pure (analysed as 1-Chloro-2,4-acetamidobenzene by liquid chromatography), is obtained in quantitative yield.

후처리

  1. customequipped with gas introduction stirrer
  2. customa temperature of 60° C
  3. custom4 hours

출처 및 근거

ORD 기록
ord-559f18dcda8a431f96929c3468782f77
출처 데이터셋
uspto-grants-1990_10
특허 번호
US04960936

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