Researchers who often do experiments know that organic synthesis is a process of preparing more complex target molecules from simple raw materials through one or more chemical reactions. Generally, it requires fewer steps, and cheap raw materials. 2106-04-9, name is 3-Chloro-2-fluoroaniline, A new synthetic method of this compound is introduced below., name: 3-Chloro-2-fluoroaniline
EXAMPLE 12(trans)-9-[4-(3-chloro-2-fluoro-phenylamino)-7-methoxy-quinazolin-6-yloxy]-1,4-diaza-spiro[5.5]undecan-5-one Process Step O12 g of the impure (trans)-9-(4-chloro-7-methoxy-quinazolin-6-yloxy)-1,4-diaza-spiro[5.5]undecan-5-one hydrochloride from the previous step are added batchwise to a solution of 3.9 g of 3-chloro-2-fluoroaniline in 60 ml of 2N hydrochloric acid at RT within 90 min. The suspension is heated to 40 C. for 60 min. Then 60 ml of toluene are added and the mixture is cooled to RT. After 50 min it is filtered and the precipitate is washed with 50 ml of toluene and 50 ml of sat. NaCl solution. After drying at 40 C., 10 g of a solid are obtained, which contains the product. The product is purified by basic chromatography on silica gel.Mass spectrum (ESI+): m/z=486 [M+H]+ 1H NMR (400 MHz, DMSO): 9.60 (1H, s); 8.37 (1H, s); 7.82 (1H, s); 7.45-7.54 (2H, m), 7.36 (1H, s); 7.28 (dt, 1H); 7.22 (1H, s); 4.63-4.67 (1H, m); 3.95 (3H, s); 3.11-3.15 (2H, m); 2.82-2.86 (2H, m); 2.30 (1H, s); 2.13-2.22 (2H, m); 1.83-1.96 (4H, m); 1.44-1.51 (2H, m).
The synthetic route of 2106-04-9 has been constantly updated, and we look forward to future research findings.
Reference:
Patent; BOEHRINGER INGELHEIM INTERNATIONAL GMBH; US2011/183987; (2011); A1;,
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