New downstream synthetic route of C7H5ClF3N

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Adding a certain compound to certain chemical reactions, such as: 69411-05-8, name is 3-Chloro-5-trifluoromethylaniline, belongs to chlorides-buliding-blocks compound, can increase the reaction rate and produce products with better performance than those obtained under traditional synthetic methods. Here is a downstream synthesis route of the compound 69411-05-8, Quality Control of 3-Chloro-5-trifluoromethylaniline

To a stirred mixture of Preparation 65A (2.51 g, 12.9 mmoL) in EtOH (130 mL) was added acetic anhydride (15.0 mL, 159 mmoL). The mixture was stirred at room temperature for 17 h. The mixture was then poured into a mixture of 40 mL of ice, 10 mL of saturated NaHCCh solution and 60 mL of EtOAc. The aqueous layer was separated and extracted with EtOAc (1 x 60 mL). The combined EtOAc layers were washed with brine (Ix 20 mL), dried (MgSO4), filtered and concentrated in vacuo to give 2.88 g of Preparation 65B in 94% yield. [00497] HPLC: 2.84 min (RT)(Chromolith SpeedROD column 4.6 x 50 mm, 10- 90% aqueous MeOH over 4 minutes containing 0.2% phosphoric acid, 4 mL/min, monitoring at 220 nm). MS (ES): m/z=238 [M+H]+. 1H NMR (400 MHz, DMSO-d6) delta ppm 10.4 (s, IH, NH) 7.96 (s, IH) 7.91 (s,l H) 7.50 (s, IH), 2.09 (s, 3H).

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Reference:
Patent; BRISTOL-MYERS SQUIBB COMPANY; WO2009/3077; (2008); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics