Continuously updated synthesis method about 39478-78-9

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Adding a certain compound to certain chemical reactions, such as: 39478-78-9, name is 5-Bromo-2-methylaniline, belongs to bromides-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 39478-78-9, HPLC of Formula: C7H8BrN

2. Synthesis of 1-(6-bromo-1H-indazol-1-yl)ethanone Into a 500 mL round-bottom flask, was placed a solution of 5-bromo-2-methylbenzenamine (25 g, 134.41 mmol) in CHCl3 (60 mL). To the above was added acetic anhydride (27.97 g, 273.95 mmol) dropwise with stirring, while cooling to a temperature of 0 C. over a time period of 1 hour. The resulting solution was allowed to react, with stirring, for 3 hours while the temperature was maintained at 0-5 C. in a bath of H2O/ice. The reaction progress was monitored by TLC (ethyl acetate/petroleum ether=1:5). Addition of isoamylnitrite (37.35 g, 319.23 mmol) was next. This was followed by the addition of KOAc (4.39 g, 44.80 mmol). To the mixture was added acetic anhydride (47.6 g, 466.21 mmol). The resulting solution was allowed to react, with stirring, overnight while the temperature was maintained at reflux in a bath of oil. The reaction progress was monitored by TLC (ethyl acetate/petroleum ether=1:5). The mixture was concentrated by evaporation under vacuum using a rotary evaporator. Adjustment of the pH to 7 was accomplished by the addition of NaHCO3 (50%). The resulting solution was extracted three times with 600 mL of ethyl acetate and concentrated by evaporation under vacuum using a rotary evaporator. The residue was purified by eluding through a column with a 1:100 ethyl acetate/petroleum ether solvent system. This resulted in 26 g (81%) of 1-(6-bromo-1H-indazol-1-yl)ethanone as a orange solid.

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Reference:
Patent; MEMORY PHARMACEUTICALS CORPORATION; US2008/200471; (2008); A1;,
Bromide – Wikipedia,
bromide – Wiktionary