Some scientific research about Diethyl 4,4-difluoroheptanedioate

Electric Literature of 22515-16-8, In the chemical reaction process, reaction time, type of solvent, can easily affect the result of the reaction, thereby determining the yield and properties of the reaction product. An updated downstream synthesis route of 22515-16-8 as follows.

Electric Literature of 22515-16-8, In the chemical reaction process, reaction time, type of solvent, can easily affect the result of the reaction, thereby determining the yield and properties of the reaction product. An updated downstream synthesis route of 22515-16-8 as follows.

General procedure: Solid, fine powdered lithiumaluminium hydride (2.0 – 5.0 equiv.) is suspended in dry THF at room temperature. The corresponding diacid- or diester derivative is dissolved in dry THF and the solution is slowly added dropwise to the lithiumaluminium slurry while cooling with an ice bath. After complete addition, the reaction solution is warmed to room temperature and the consumption of the starting material is checked by TLC. The suspension is carefully quenched with 2M H2SO4, additional water is added. For a better workup, the suspension should have a pH of ~7. The phases are separated and extracted with Et.20. The organic phase is washed with H2O, dried over MgSO4 and evaporated under reduced pressure. The crude product is directly used without further purification or purified via column chromatography using cyclohexane / tert. -butyl methyl ether. 1H NMR (500 MHz, CDCIs) delta 3.70 (t, 4H, J = 6.3 Hz), 2.00-1 .90 (m, 4H), 1 .79-1 .74 (m, 4H), 1 .38 (br s, 2H).

According to the analysis of related databases, 22515-16-8, the application of this compound in the production field has become more and more popular.

Reference:
Patent; MERCK PATENT GMBH; SCHRAUB, Martin; DOBELMANN-MARA, Lars; RIEDMUELLER, Stefan; (326 pag.)WO2018/149852; (2018); A1;,
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