A kind of synthetic method of dehydrodunglitol intermediate
A kind of technology of dehydrated dulcitol and synthesis method, applied in directions such as organic chemistry, introduction of halogen preparation, etc., can solve problems such as dangerous operation process, complicated process, etc., achieve yield and purity improvement, safe and reasonable process, and high yield. Effect
- Summary
- Abstract
- Description
- Claims
- Application Information
AI Technical Summary
Problems solved by technology
Method used
Image
Examples
Embodiment 1
[0037] Get 10kg of dulcitol and put it in the reaction kettle, add 15 times of the weight of dulcitol and a hydrobromic acid solution with a concentration of 40%, heat it in a water bath to 70°C, keep it warm and react with constant stirring for 15 hours, feed nitrogen to pressurize during the reaction, The range of pressurization with the reaction time is: 0-1 hour, the pressure is gradually increased from 0MPa to 0.1MPa; 1-5 hours, the pressure is gradually increased from 0.1MPa to 0.5MPa; 5-9 hours, the pressure is gradually increased from 0.5MPa to 0.9 MPa; 9-15 hours, the pressure is gradually increased from 0.9MPa to 1.4MPa; the reaction is completed to obtain a dibromodulcitol solution; the dibromodulcitol solution is left to stand at room temperature for 24 hours, and filtered to obtain a dibromodulcitol coarse crystal Add 100 times the weight of methanol to the crude crystals of dibromodulcitol, and recrystallize at 2°C to obtain dibromodulcitol.
[0038] Experimental...
Embodiment 2
[0040] Take 10kg of dulcitol and put it in a reaction kettle, add a hydrobromic acid solution with 2 times the weight of dulcitol and a concentration of 20%, heat it in a water bath to 30°C, keep it warm and stir continuously for 2 hours, during the reaction, argon gas is introduced to pressurize , the pressurization range with the reaction time is: 0-1 hour, the pressure is gradually increased from 0MPa to 0.05MPa; 1-2 hours, the pressure is gradually increased from 0.05MPa to 0.1MPa; The dulcitol solution was allowed to stand at room temperature for 12 hours, filtered to obtain crude crystals of dibromodulcitol; the crude crystals of dibromodulcitol added methanol 80 times the weight of the crude crystals, and recrystallized at 6°C to obtain dibromodulcitol alcohol.
[0041] Experimental results: The average yield of dibromodunglitol is 50%, and the average purity is 80%.
Embodiment 3
[0043] Take 10kg of dulcitol and put it in a reaction kettle, add 6 times the weight of dulcitol and a hydrobromic acid solution with a concentration of 30%, heat it in a water bath to 90°C, keep it warm and stir continuously for 8 hours, during the reaction, helium gas is introduced to pressurize , the range of pressurization with the reaction time is: 0-1 hour, the pressure is gradually increased from 0MPa to 0.1MPa; 1-4 hours, the pressure is gradually increased from 0.1MPa to 0.3MPa; 4-8 hours, the pressure is gradually increased from 0.3MPa to 0.5MPa; the reaction is completed to obtain a dibromodulcitol solution; the dibromodulcitol solution is allowed to stand at room temperature for 30 hours, and filtered to obtain a dibromodulcitol coarse crystal; the dibromodulcitol coarse crystal adds 70 times the weight of the coarse crystal Methanol was recrystallized at 8°C to obtain dibromodulcitol.
[0044] Experimental results: The average yield of dibromodulcitol is 53%, and ...
PUM
Login to View More Abstract
Description
Claims
Application Information
Login to View More