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2-acetyl benzimidazolyl-glycin schiff base preparation method

A technology of acetyl benzimidazole glycine Schiff base and acetyl benzimidazole is applied in the field of preparation of 2-acetyl benzimidazole glycine Schiff base, and can solve the problem of long reaction time and less than 90% Yield, serious pollution in the reaction process, etc.

Inactive Publication Date: 2007-05-30
NORTHWEST UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] ①The reaction takes a long time and the yield is not high. By reproducing the synthesis steps reported in the literature and prolonging the reaction time, the reported yield cannot reach 63%, but only about 30%.
[0007] ②The reaction process of this synthesis method has serious pollution and is difficult to synthesize in large quantities
[0009] The solubility in n-hexane, the recrystallization solvent used, is very poor. The product recrystallized in 300ml of hot n-hexane is less than 1g. The waste of reagents is very large, and the recrystallization efficiency is very low, which is far less than 90% of its reported value. Yield, only about 60%

Method used

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  • 2-acetyl benzimidazolyl-glycin schiff base preparation method

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Experimental program
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Embodiment 1

[0019] Embodiment 1 The synthetic method of precursor 2-acetylbenzimidazole

[0020] Step 1: Synthesis of 2-(1'-hydroxyethyl)benzimidazole:

[0021]

[0022] In a 100ml three-neck flask, dissolve 10g of o-phenylenediamine in 25ml of 4mol / L HCl, stir until completely dissolved, adjust the pH to 2 with HCl, and then add 0.1g of catalyst FeCl 3 ·6H 2 O and 13ml lactic acid, heated to reflux for 4 hours, cooled, slowly added solid Na 2 CO 3 Neutralize the powder and stir vigorously until the pH is close to 7, then add 20% Na 2 CO 3 Adjust until the solution changes from black-red to yellow-green, and a large amount of precipitates are formed, which is left to stand and filtered with suction to obtain the crude product. Recrystallize directly with water, add activated carbon for decolorization, filter while hot, and precipitate 13.5 g of white crystals after cooling, with a yield of 80% and a melting point of 180.4-181.0°C (literature value of 177-179°C).

[0023] Step 2: ...

Embodiment 2

[0025] Example 2 Preparation of 2-acetyl benzimidazole glycine Schiff base

[0026] Glycine (0.7507g, 0.01mol) and KOH (0.56g, 0.01mol) were dissolved in 25mL of methanol, stirred for about 15 minutes until dissolved, filtered, and 2-acetylbenzo Imidazole (1.602g, 0.01mol) in 20mL of methanol solution, after reflux for 5-14 hours, the color of the solution changed from yellow to dark brown red, part of the methanol was evaporated, cooled, a precipitate formed, suction filtered, washed with methanol and chloroform respectively, Dry it under infrared light, place it in a concentrated sulfuric acid desiccator to obtain a khaki powder.

[0027] 1 H NMR hydrogen spectrum (400MHz, CD 3 OD): δ7.6(q, 2H, a Coupling peak on H-Ar), δ7.3(q, 2H, b Coupling peak on H-Ar), δ5.311 (d, 1H, H-N), δ2.582 (s, 2H, -CH 2 -), δ1.652(s, 3H, CH 3 ).

[0028] Infrared (cm -1 )(KBr) 1643(C=N), 1570(ν as COO - ), 1428 (ν s COO - )

[0029] Raman (cm -1 ): 1644.76 (C=N), 1566.93ν as COO -...

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Abstract

The invention discloses a making method of 2-acetyl benzimidazole glycine Schiff base, which relates to the synthesis of 2-(1'-hydroxy ethyl) benzimidazole, prosoma 2-acetyl benzimidazole and 2-acetyl benzimidazole glycine Schiff base.

Description

[0001] The application date of this patent is: June 1, 2005, the application number is: 200510042748.9, and the invention name is: 2-acetylbenzimidazole glycine Schiff base rare earth complex and its preparation method. Apply. technical field [0002] The invention relates to a preparation method of 2-acetyl benzimidazole glycine Schiff base. Background technique [0003] Rare earth amino acid complexes have been one of the hotspots of people's research because of their wide use in agriculture and medicine. Rare earth ions have a similar ionic radius to the life metal element calcium, and the unique fluorescence properties of rare earth ions due to the existence of 4f electrons can be used as probes to reveal Na + 、K + , Ca 2+ Therefore, the depth and breadth of research in this area are increasing day by day. However, due to the Na in the living system + 、K + , Ca 2+ The coordination environment of the plasma is very complicated, and its function is not only reflecte...

Claims

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Application Information

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IPC IPC(8): C07D235/12C07F5/00
Inventor 杨一心王党辉赵天成李青翠陈冬梅
Owner NORTHWEST UNIV