In the next few decades, the world population will flourish. As the population grows rapidly and people all over the world use more and more resources, all industries must consider their environmental impact. 685-88-1, name is Diethyl fluoromalonate belongs to esters-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. Quality Control of Diethyl fluoromalonate
2-fluoromalonic acid diethylester is manufactured from 2-chloromalonic acid diethylester and l,8-diazabicyclo[5,4,0]undec-7-ene- l,37HF neat at 80C, as described in example 2 of US 7,145,046. The raw product is hydrolyzed, in analogy to example 1 of DE-Offenlegungsschrift 4120704, by contacting it with NaOH in water (concentration of NaOH : 30% by weight). Resulting ethanol is removed by distillation, and the resulting solution is contacted withLewatit S 100 in the H-form (i.e. comprising acidic H+). The aqueous solution of fluoromalonic acid is mixed with toluene, and at a reduced pressure(400 mbar), a water/toluene mixture is removed.The resulting fluoromalonic acid then reacted with acetone as described by D. Davidson and S. A. Bernhard in J. Chem. Soc. 70(1948), page 3428, 1. paragraph in chapter “Experimental”. The fluoromalonic acid is suspended in acetic anhydride and concentrated sulfuric acid is added. The amounts of the reagents and starting compounds correspond to those described by Davidson et al.The acetone is added under cooling. After a post-reaction phaseof 2 hours, 5-fluoro-2,2-dimethyl-l,3-dioxane-4,6-dione can be isolated.
The synthetic route of 685-88-1 has been constantly updated, and we look forward to future research findings.
Reference:
Patent; SOLVAY SA; BRAUN, Max Josef; WO2013/79397; (2013); A1;,
Ester – Wikipedia,
Ester – an overview | ScienceDirect Topics