Reference of 432-21-3, 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 432-21-3 as follows.
To a stirred solution of chloral hydrate (2.54 g, 15.3 mmol) in H20 (30 ml) was addedNa2S04 (0.87 g, 6.14 mmol) and 3-chloro-2-(trifluoromethyl)aniline (2.00 g, 10.2 mmol)followed by addition of NH20H.HCI (2.13 g, 30.7 mmol) at room temperature. The reactionmixture was heated at 55C for 16h. Progress of reaction was monitored by TLC and5 LCMS. After completion, the reaction mixture was diluted with H20 (1 00 ml) andextracted with EtOAc (2 x 40 ml). The organic layer was separated, dried over anhydrousNa2S04 and concentrated under vacuum. The crude obtained was purified by combi-flashchromatography (10 to 20% EtOAc in hexanes) to (E)-N-(3-chloro-2-(trifluoromethyl)phenyl)-2-(hydroxyimino)acetamide Xl-16a (1.25 g) as an off-white solid.10 Yield: 44%.Basic LCMS Method 2 (ES-): 265 (M-H)-, 97 % purity.1H NMR (400 MHz, DMSO-d5) o 7.48 (d, J=7.82 Hz, 1 H) 7.61 (s, 1 H) 7.62-7.68 (m, 2H)10.10 (s, 1H) 12.36 (s, 1H).
According to the analysis of related databases, 432-21-3, the application of this compound in the production field has become more and more popular.
Reference:
Patent; UCB PHARMA GMBH; MUELLER, Christa E.; PEGURIER, Cecile; DELIGNY, Michael Louis Robert; EL-TAYEB, Ali; HOCKEMEYER, Joerg; LEDECQ, Marie; MERCIER, Joel; PROVINS, Laurent; BOSHTA, Nader M.; BHATTARAI, Sanjay; NAMASIVAYAM, Vigneshwaran; FUNKE, Mario; SCHWACH, Lukas; GOLLOS, Sabrina; VON LAUFENBERG, Daniel; BARRE, Anais; (493 pag.)WO2018/122232; (2018); A1;,
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