Nitric Acid → HCID 15291316, 화합물

HRID 1654482노트

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HRID 1654482 반응식
[Cl:1][C:2]1[CH:20]=[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+:21]([O-])([OH:23])=[O:22].O.[OH-].[Na+]>S(=O)(=O)(O)O>[Cl:1][C:2]1[C:20]([N+:21]([O-:23])=[O:22])=[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

참가 물질

6

반응물 4

HCID 944Nitric AcidHCID 962WaterHCID 14798Sodium HydroxideHCID 20078040HCID 20078040, 화합물

생성물 1

HCID 15291316HCID 15291316, 화합물수율 91.7%

시약·촉매·용매 1

HCID 1118Sulfuric Acid용매2회

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온도
0 °C

실험 절차

5-Chloro-1-isopropyl-2-(4-methyl-1-piperazinyl)benzimidazole (24.1 g) was dissolved in concentrated sulfuric acid (160 ml). To the solution were added dropwise concentrated nitric acid (7.8 g) and concentrated sulfuric acid (20.2 g) at 0° C. and the mixture was stirred at 0° C. for 5 minutes. The reaction mixture was poured into water and the mixture was made basic with an aqueous sodium hydroxide solution 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 to give 5-chloro-1-isopropyl-2-(4-methyl-1-piperazinyl)-6-nitrobenzimidazole (25.5 g). A part of the obtained product was recrystallized from acetonitrile, which showed the physical properties consistent with those in Preparation 8.

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

출처 및 근거

ORD 기록
ord-6af057016719492e8d22723c5bb26d2e
출처 데이터셋
uspto-grants-1995_04
특허 번호
US05407936

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