Benzimidazolone compound
A technology of benzimidazolone and compound, applied in the field of benzimidazolone compound, can solve problems such as difficulty in color tone
- Summary
- Abstract
- Description
- Claims
- Application Information
AI Technical Summary
Problems solved by technology
Method used
Image
Examples
Embodiment 1
[0069] To 750 parts of 1,3-dimethyl-2-imidazolidinone, 43.6 parts of 5-aminobenzimidazolone, 30 parts of dimethylsuccinyl succinate and 13.4 parts of concentrated sulfuric acid were added, and The resulting mixture was heated at 180°C for 14 hours. Then cool to room temperature, filter the deposit, wash with 200 parts of 1,3-dimethyl-2-imidazolidinone and 600 parts of acetone to remove impurities, and then dry at 110° C. under reduced pressure for 8 hours, thus obtaining 17.7 parts (28% yield) of bright red colored α-form crystals. When these red α-form crystals were analyzed by infrared spectroscopy and field desorption mass spectrometry (FD-MS), the following results were obtained.
[0070] IR
[0071] Infrared spectrum analysis using a Fourier transform infrared spectrophotometer FT / IR-550 manufactured by Jasco Corporation showed absorption peaks due to stretching vibrations as follows:
[0072] 3200cm -1 : N-H stretching vibration of the amide group within the imidazol...
Embodiment 2
[0087] To 10 parts of N,N-dimethylformamide was added 2 parts of the red α-type crystal obtained in Example, and the mixture was heated at 90° C. for 6 hours. The resulting mixture was then cooled to room temperature, the slurry was filtered, and washed with 50 parts of acetone, and the resulting deposit was dried under reduced pressure at 110° C. for 8 hours, thus obtaining 1.6 parts (yield 80%) of bright yellow colored β type crystal.
[0088] These yellow β-form crystals were analyzed by powder X-ray diffraction using the same method as described for the red α-form crystals obtained in Example 1. The obtained X-ray diffraction pattern is shown in FIG. 2 . It was shown that this crystal is different from the α-type crystal, and exhibits Cu-Kα characteristic X-ray diffraction peaks at Bragg angles 2θ of 14.3±0.2°, 16.6±0.2°, 24.2±0.2°, and 24.8±0.2°.
Embodiment 3
[0090] 15 parts of the red α-type crystal obtained in Example 1, 150 parts of common salt, and 37.5 parts of diethylene glycol were mixed together and ground in a kneader. The resulting mixture was then peptized in 1000 parts of water at 60°C, followed by filtration. The washing process in which the wet cake thus obtained was peptized in 1000 parts of water at 60°C was repeated 3 times and then filtered. The resulting washed wet cake was then dried at 110° C. under reduced pressure for 8 hours, thereby obtaining 13.5 parts (yield 90%) of bright red-purple colored γ-form crystals.
[0091] These yellow β-form crystals were analyzed by powder X-ray diffraction using the same method as described for the red α-form crystals obtained in Example 1. The obtained X-ray diffraction pattern is shown in FIG. 3 . Diffraction of X-rays showing that this crystal is different from α-type crystals and exhibits Cu-Kα characteristics at Bragg angles 2θ of 9.9±0.2°, 14.3±0.2°, 16.3±0.2°, 24.5±...
PUM
Login to View More Abstract
Description
Claims
Application Information
Login to View More