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

HRID 1654484노트

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HRID 1654484 반응식
[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

참가 물질

5

반응물 2

HCID 222AmmoniaHCID 15291316HCID 15291316, 화합물

생성물 1

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

시약·촉매·용매 2

HCID 23994Zinc촉매HCID 313Hydrochloric Acid용매

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온도
80 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-9dfa155afd594b38a1759cd62cfa4652
출처 데이터셋
uspto-grants-1995_04
특허 번호
US05407936

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