Electric Literature of 13534-98-0, 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. 13534-98-0, name is 4-Amino-3-bromopyridine. A new synthetic method of this compound is introduced below.
General procedure: A mixture of amino pyridine 1 (1.0 mmol), 10%Pd/C (0.010 mmol), CuI (0.010 mmol), PPh3 (0.022 mmol) and Cs2CO3 (3 mmol) in PEG-400 (3 mL) was stirred for 15 min at room temperature under a nitrogen atmosphere. To this was added an appropriate iodoarene 2 (1.0 mmol) and the mixture was stirred further for 10 min. The mixture was then stirred at 95 – 100 C for 2.5 h under ultrasound irradiation using a laboratory ultrasonic bath Sonorex Super RK 510H model producing irradiation of 35 kHz. After cooling the mixture to room temperature an appropriate terminal alkyne 3 (1.2 mmol) was added to it. The mixture was then stirred again at 95-100 C for 4h under ultrasound irradiation. After completion of the reaction (indicated by TLC), the mixture was diluted with cold water (30 mL) and extracted with CH2Cl2 (3 x 10 mL). The organic layers were collected, combined, washed with cold water (2 x 15 mL), dried over anhydrous Na2SO4, filtered and concentrated under reduced pressure. The crude product was then purified by column chromatography on silica gel using EtOAc / n-hexane as a solvent system.
At the same time, in my other blogs, there are other synthetic methods of this type of compound,13534-98-0, 4-Amino-3-bromopyridine, and friends who are interested can also refer to it.
Reference:
Article; Dandela, Rambabu; Nath Singh, Shambhu; Pal, Manojit; Ramamohan, Hindupur; Siddaiah, Vidavalur; Venkateshwarlu, Rapolu; Tetrahedron Letters; (2019);,
Pyridine – Wikipedia,
Pyridine | C5H5N – PubChem