344-19-4, 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 344-19-4 as follows.
2,6-dichloro-4-fluoro-aniline (12 g, 67 mmol) was taken up in concentrated H0I (13 mL)and water (Si mL) at 0 00 After stirring for iS mm, a solution of NaNO2 (4.85 g, 70.3 mmol) in 147water (10 mL) was added drop-wise at 0 00 and the mixture was stirred for 45 mm. A solution of MeSNa (35 g, 100 mmol) and Na2CO3 (10.6 g, 100 mmol) in water (100 mL) was then added to the above solution drop-wise at 50 00. After addition, the mixture was stirred for 1 hour, then extracted with Et0Ac and the combined organic layers were dried (MgS04), filtered and thefiltrate concentrated in vacuo to give the crude product. Flash chromatography using neat 60-90 petrol ether afforded 1 ,3-d ichloro-5-fluoro-2-methylsulfanyl-benzene (4.7 g, 34%).1H NMR (ODd3, 400MHz): 57.17 (d, 2H), 2.41 (s, 3H).
According to the analysis of related databases, 2,6-Dichloro-4-fluoroaniline, the application of this compound in the production field has become more and more popular.
Reference:
Patent; BASF SE; CALO, Frederick; KORDES, Markus; KRAUS, Helmut; MIETZNER, Thomas; SEITZ, Thomas; KREUZ, Klaus; PASTERNAK, Maciej; NEWTON, Trevor William; MASSA, Dario; WO2015/7564; (2015); A1;,
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