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 18282-59-2 as follows. Quality Control of 4-Bromo-1,2-dichlorobenzene
A. 1-Bromo-4,5-dichloro-2-nitro-benzene. 4-Bromo-1,2-dichlorobenzene (10.5 g, 46.3 mmol) was added to 25 mL concentrated sulfuric acid at 0° C. A 1:1 mixture of 70percent nitric acid and concentrated sulfuric acid (20 mL) was added dropwise over 40 min. The reaction mixture was allowed to warm to ambient temperature with stirring over 0.5 h, then was poured onto cracked ice. The resulting mixture was filtered through paper, and the collected solids were washed with water (5*) and then dried at 45° C. under reduced pressure for 30 min to provide 10.7 g of an 88:12 mixture of desired nitroarene to starting material. Recrystalization from absolute ethanol provided 4.76 g of long yellow needles corresponding to a 20:1 mixture of product to starting material. The mother liquor was concentrated and recrystallized twice to provide an additional 1.18 g of product (17:1 mixture with recovered starting material). TLC (silica gel, 1:1 hexanes/EtOAc): Rf=0.45. 1H NMR (400 MHz, CDCl3): 7.95 (s, 1H), 7.80 (s, 1H).
According to the analysis of related databases, 18282-59-2, the application of this compound in the production field has become more and more popular.
Reference:
Patent; Allison, Brett; McAtee, Laura C.; Phuong, Victor K.; Rabinowitz, Michael H.; Shankley, Nigel P.; US2004/224983; (2004); A1;,
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