Ammonia → 1H-Benzimidazol-6-amine, 5-chloro-1-(1-methylethyl)-2-(4-methyl-1-piperazinyl)-

HRID 1654484ノート

反応式

HRID 1654484 の反応式
[Cl:1][C:2]1[C:20]([N+:21]([O-])=O)=[CH:19][C:5]2[N:6]([CH:16]([CH3:18])[CH3:17])[C:7]([N:9]3[CH2:14][CH2:13][N:12]([CH3:15])[CH2:11][CH2:10]3)=[N:8][C:4]=2[CH:3]=1.N>Cl.[Zn]>[NH2:21][C:20]1[C:2]([Cl:1])=[CH:3][C:4]2[N:8]=[C:7]([N:9]3[CH2:14][CH2:13][N:12]([CH3:15])[CH2:11][CH2:10]3)[N:6]([CH:16]([CH3:18])[CH3:17])[C:5]=2[CH:19]=1

参加物

5

反応物 2

HCID 222AmmoniaHCID 15291316HCID 15291316、化合物

生成物 1

HCID 30732911H-Benzimidazol-6-amine, 5-chloro-1-(1-methylethyl)-2-(4-methyl-1-piperazinyl)-収率 54.9%

試薬・触媒・溶媒 2

HCID 23994Zinc触媒HCID 313Hydrochloric Acid溶媒

反応条件

温度
80 °C

実験手順

5-Chloro-1-isopropyl-2-(4-methyl-1-piperazinyl)-6-nitrobenzimidazole (1.2 g) was dissolved in 2.5N hydrochloric acid (20 ml) and thereto was added zinc powder (1.5 g) in portions and the mixture was stirred at 80° C. for 4 hours. The reaction mixture was made basic with an aqueous ammonia and extracted with chloroform. The chloroform layer was washed with water and dried over anhydrous magnesium sulfate and then the solvent was distilled off under reduced pressure. The residue was recrystallized from acetonitrile to give 6-amino-5-chloro-1-isopropyl-2-(4-methyl-1-piperazinyl)benzimidazole (0.6 g) as colorless crystal.

後処理

  1. extractionextracted with chloroform
  2. washThe chloroform layer was washed with water
  3. dry with materialdried over anhydrous magnesium sulfate
  4. distillationthe solvent was distilled off under reduced pressure
  5. customThe residue was recrystallized from acetonitrile

出典と根拠

ORDレコード
ord-9dfa155afd594b38a1759cd62cfa4652
出典データセット
uspto-grants-1995_04
特許番号
US05407936

反応ノート

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