Discovery of 626-40-4

The basis of chemical reaction formula synthesis, the synthesis route is composed of some specific reactions and combined according to certain logical thinking. We look forward to the emergence of more reaction modes in the future.

Researchers who often do experiments know that organic synthesis is a process of preparing more complex target molecules from simple raw materials through one or more chemical reactions. Generally, it requires fewer steps, and cheap raw materials. 626-40-4, name is 3,5-Dibromoaniline, A new synthetic method of this compound is introduced below., Computed Properties of C6H5Br2N

This compound was preparedwithout the use of air and moisture sensitive protocol. Using a modifiedpreparation similar to that used by Kln and co-workers[1], aqueousformaldehyde (37%, 31.2 mL) was added to a stirring mixture of THF (300 mL)and 3M H2SO4 (84 mL) cooled to 0C in a 1 L long neck flat bottom flask. After stirring for 10minutes at 0C, 3,5 dibromoaniline (35.00 g, 139.5 mmol) dissolved in THF (75mL) was addeddropwise over 15 minutes. The solution was stirred for another 10 minutes at 0C. This mixturewas then stirred vigorously while NaBH4 (21.14 g, 558.8 mmol) was carefully added portionwiseover a period of 30 minutes at 0C. After stirring at room temperature for 2 hours the solutionwas filtered and the solid was washed with THF (30 mL). The filtrate was collected and allvolatiles were removed via rotary evaporation. The remaining residue was basified withsaturated aqueous NaHCO3 (500 mL) and extracted with dichloromethane (3 x 100 mL). Theorganic extracts were combined, washed with water (200 mL), dried with anhydrous MgSO4 andfiltered. All volatiles were removed from the filtrate via rotary evaporation and an orange-redsolid was obtained in 96 % yield (37.51 g, 134.5 mmol). Material was used without furtherpurification.

The basis of chemical reaction formula synthesis, the synthesis route is composed of some specific reactions and combined according to certain logical thinking. We look forward to the emergence of more reaction modes in the future.

Reference:
Article; Smith, Joel D.; Chih, Edwina; Piers, Warren E.; Spasyuk, Denis M.; Polyhedron; vol. 155; (2018); p. 281 – 290;,
Bromide – Wikipedia,
bromide – Wiktionary