In the next few decades, the world population will flourish. As the population grows rapidly and people all over the world use more and more resources, all industries must consider their environmental impact. 1003-99-2, name is 2-Bromo-5-fluoroaniline belongs to bromides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. Quality Control of 2-Bromo-5-fluoroaniline
Dissolve 2-bromo-5-fluoroaniline (25g, 131 mmol) in methyldisulfide (220 mL) and heat to 75 ¡ãC under nitrogen. Add isoamyl nitrite (46 mL, 342 mmol) dropwise via an addition funnel trough a reflux condenser (-1 drop/sec). Large exotherm may occur if addition is too fast. After addition is complete heat the reaction to 95 ¡ãC for 1 hour and cool to room temperature and concentrate in vacuo. Purify residue twice via silica gel chromatography eluting with hexanes to yield 22 g of 1-bromo-4-fluoro-2-methylsulfanyl- benzene (76percent). Dissolve l-bromo-4-fluoro-2-methylsulfanyl-benzene (22 g, 99.6 mmol) in dry THF (500 mL) and cool to-78 ¡ãC under nitrogen. Add butyl lithium (2. 5M in hexanes, 48 mL, 120 mmol) slowly and stir for 10 minutes after complete addition. Add trimethyl borate (22 mL, 200 mmol) and warm to room temperature. Pour into 0.1 M NaOH and extract with ether. Acidify the aqueous layer to pH 2 with concentrated HC1. Extract with ether, rry the organic layer with sodium sulfate, filter and concentrate in vacuo to yield 15.4 g (83percent) of the title compound.
The synthetic route of 1003-99-2 has been constantly updated, and we look forward to future research findings.
Reference:
Patent; ELI LILLY AND COMPANY; WO2005/73204; (2005); A1;,
Bromide – Wikipedia,
bromide – Wiktionary