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

HRID 1087993

反応式

HRID 1087993 の反応式
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]

参加物

7

反応物 4

HCID 61-Chloro-2,4-DinitrobenzeneHCID 176Acetic AcidHCID 9864Cyanamide2 回HCID 160693Formamidine acetate

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

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.

後処理

  1. customequipped with gas introduction stirrer
  2. customa temperature of 25° C.
  3. customa temperature of 60° C

出典と根拠

ORDレコード
ord-854f343b508f4d689cd02c64dc88fc11
出典データセット
uspto-grants-1990_10
特許番号
US04960936

関連ノート

読み込み中…