1003-99-2, name is 2-Bromo-5-fluoroaniline, belongs to bromides-buliding-blocks compound, is considered to be a conventional heterocyclic compound, which is widely used in drug synthesis. The chemical synthesis route is as follows. name: 2-Bromo-5-fluoroaniline
1-(5-fluoroquinolin-8-yl)piperidin-4-one (Example P, Step 3) is also prepared as shown in the reaction scheme above. To a 500 ml flask equipped with a stirrer, a thermocouple, a condenser and nitrogen inlet were charged 50 g 2-bromo-5-fluoroaniline and 60 g glycerol. The mixture was heated to 60¡ã C. and 55 g nitrobenzene sulfonic acid was charged in portion. The mixture was then heated to 100-110¡ã C., started charge 200 ml 70percent sulfuric acid. After sulfuric acid addition, the mixture was heat to 130¡ã C. and stirred for 3 hours before cooled to room temperature. Water (300 g) was added and a grayish by product was filtered off. The filtrate was slowly added into a 2-L reactor containing a mix of 420 g 50percent NaOH, 420 g of water, 352 g methyl tert-butyl ether. After filtering off small amount solid, the aqueous layer was split off and the organic layer was washed with 10percent NaOH (2.x.100 ml), 20percent NaCl (2.x.200 ml), the solvent was removed, weight 56 g, 89.8percent.
The synthetic route of 1003-99-2 has been constantly updated, and we look forward to future research findings.
Reference:
Patent; Wyeth; US2007/27160; (2007); A1;,
Bromide – Wikipedia,
bromide – Wiktionary