Method for synthesizing 2-bromo-4-nitroimidazole
A technology of nitroimidazole and bromine, applied in the field of synthesis of 2-bromo-4-nitroimidazole, can solve problems such as high price, long treatment time, residual heavy metal elements, etc., and is beneficial to industrialized production and reaction chemical selection. Good performance and mild reaction conditions
- Summary
- Abstract
- Description
- Claims
- Application Information
AI Technical Summary
Problems solved by technology
Method used
Image
Examples
Embodiment 1
[0031] Embodiment 1: Preparation of 2,5-dibromo-4-nitroimidazole
[0032] In a 20L reaction kettle equipped with mechanical stirring, reflux condenser and tail gas receiving device, add 4-nitroimidazole (1500g), distilled water (13L), sodium bicarbonate (2458g) respectively, stir, and control the temperature at 25 Bromine (1565 mL) was added dropwise within ℃. After the dropwise addition, raise the temperature to 50-55°C and continue stirring until the reaction is complete, stop heating, cool down to 5°C, and filter. The obtained solid was washed twice with distilled water and dried in vacuum to obtain 3198 g of yellow solid 2,5-dibromo-4-nitroimidazole.
Embodiment 2
[0033] Embodiment 2: Preparation of 2-bromo-5-iodo-4-nitroimidazole
[0034] In a 10-liter reactor equipped with mechanical stirring and reflux condensing device, add respectively 2,5-dibromo-4-nitroimidazole (1112g), sodium iodide (615g) and 6L distilled water and DMF mixed solution ( 4:1). Heat to reflux until the reaction is complete, cool to 5°C, filter, wash with distilled water twice, and dry in vacuum to obtain 1193 g of yellow solid 2-bromo-5-iodo-4-nitroimidazole.
Embodiment 3
[0035] Embodiment 3: Preparation of 2-bromo-4-nitroimidazole 11
[0036] In a 10-liter reactor equipped with mechanical stirring and reflux condenser, 2-bromo-5-iodo-4-nitroimidazole (1907 g) and absolute ethanol (3 L) were added respectively. Stir, slowly add diethyl phosphite (773mL), heat to reflux for 6 hours, evaporate most of the ethanol, cool to room temperature, add 1800mL concentrated ammonia water and 800g crushed ice, stir, then slowly add concentrated hydrochloric acid to adjust the pH to weak acidity, Cool to 5°C, filter, wash the filtered solid with distilled water, and vacuum-dry to obtain 1084 g of light yellow solid 2-bromo-4-nitroimidazole. 1HNMRδppm (400MHz, DMSO-d 6 ): 14.14(br,1H), 8.44(s,1H).
PUM

Abstract
Description
Claims
Application Information

- R&D Engineer
- R&D Manager
- IP Professional
- Industry Leading Data Capabilities
- Powerful AI technology
- Patent DNA Extraction
Browse by: Latest US Patents, China's latest patents, Technical Efficacy Thesaurus, Application Domain, Technology Topic, Popular Technical Reports.
© 2024 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap|About US| Contact US: help@patsnap.com