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

HRID 1087992

反応式

HRID 1087992 の反応式
[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(NC=NCCCC)CCC.[H][H]>[Ni].CO>[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([NH2:8])=[CH:4][C:3]=1[NH2:11]

参加物

6

反応物 3

HCID 61-Chloro-2,4-DinitrobenzeneHCID 86744256HCID 86744256、化合物HCID 178418361HCID 178418361、化合物

生成物 1

HCID 212094-Chloro-M-phenylenediamine

試薬・触媒・溶媒 2

HCID 935Nickel触媒HCID 887Methanol溶媒

実験手順

40.8 g of 1-chloro-2,4-dinitrobenzene, 2 g of Raney nickel (60%, aqueous), 2.3 g of N,N'-dibutylformamidine 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, 97% pure (analysed as 1-Chloro-2,4-acetamidobenzene by liquid chromatography), is obtained in quantitative yield.

後処理

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

出典と根拠

ORDレコード
ord-45196dd3922c46828428291de1cdc84c
出典データセット
uspto-grants-1990_10
特許番号
US04960936

関連ノート

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