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

HRID 1087993

반응식

HRID 1087993 반응식
N#CN.C(O)(=O)C.C(O)(=O)C.C(N)=N.[Cl:15][C:16]1[CH:21]=[CH:20][C:19]([N+:22]([O-])=O)=[CH:18][C:17]=1[N+:25]([O-])=O>[Ni].CO>[Cl:15][C:16]1[CH:21]=[CH:20][C:19]([NH2:22])=[CH:18][C:17]=1[NH2:25]

참가 물질

7

반응물 4

HCID 61-Chloro-2,4-DinitrobenzeneHCID 176Acetic AcidHCID 9864Cyanamide2회HCID 160693Formamidine acetate

생성물 1

HCID 212094-Chloro-M-phenylenediamine

시약·촉매·용매 2

HCID 935Nickel촉매HCID 887Methanol용매

실험 절차

1.5 g of cyanamide, 1.5 g of acetic acid, 2 g of Raney nickel (60%, aqueous), and 120 ml of methanol are introduced in an autoclave equipped with gas introduction stirrer. Under a hydrogen pressure of 4 bar and a temperature of 25° C., the cyanamide is hydrogenated quantitatively to the formamidine acetate. 40.8 g of 1-chloro-2,4-dinitrobenzene are then added to the autoclave, and the hydrogenation is carried out at a pressure of 10 bar and a temperature of 60° C. The hydrogenation time is 1 hour. 1-Chloro-2,4-diaminobenzene, 97.5% 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 25° C.
  3. customa temperature of 60° C

출처 및 근거

ORD 기록
ord-854f343b508f4d689cd02c64dc88fc11
출처 데이터셋
uspto-grants-1990_10
특허 번호
US04960936

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