Synthetic Route of 6959-48-4 ,Some common heterocyclic compound, 6959-48-4, molecular formula is C6H7Cl2N, its traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc., below Introduce a new synthetic route.
A suspension of calixarene 1 (0.17 g, 0.40 mmol), K2CO3(1.77 g, 12.8 mmol) and 3-(chloromethyl)pyridine hydrochloride (0.52 g, 3.2 mmol) in anhydrous CH3CN (10 ml) was stirred under nitrogen at 508C for 20 h. The reaction mixture was quenched with water and the residue was collected by filtration, dissolved in CH2Cl2 and washed withaNa2CO3 solution. The organic solvent was removed under reduced pressure and the residue was purified by column chromatography (SiO2;CH2Cl2 to CH2Cl2/ CH3OH, 95:5). The pure final product was obtained with a 51% yield (0.13 g).1H NMR (CDCl3,278C, 500 MHz): d 8.77 (s, 2H, H8),8.63 (d, J 5.0 Hz, 2H, H11), 8.06 (d, J 7.7Hz,2H, H9),7.57 (s, 2H, H6), 7.25 (dd, J1 7.7Hz, J2 5.0Hz, 2H, H10), 7.09 (d, J 7.6Hz, 4H, H4), 6.83 (d, J 7.6 Hz, 4H, H2), 6.71 (t, J 7.6 Hz, 4H, H1, H3),5.08 (s, 4H, H7), 4.26 (d, J 13.0 Hz, 4H, H5ax), 3.38 (d, J 13.0 Hz, 4H, H5eq). 13CNMR (CDCl3,278C, 125MHz): d 153.10, 151.51, 149.69, 148.78, 135.44,133.00, 132.25, 129.21, 128.58, 127.79, 125.77, 123.93, 119.25, 75.71, 31.41. ESI-MS: m/z 607 [M H], 629 [M Na]. UV- vis absorption (CH3CN, l268 nm): 1 7275M21 cm 21
In the field of chemistry, the synthetic routes of compounds are constantly being developed and updated. I will also mention this compound in other articles. 6959-48-4, 3-(Chloromethyl)pyridine hydrochloride, other downstream synthetic routes, hurry up and to see.
Reference:
Article; Bonaccorso, Carmela; Nicoletta, Francesca; Zito, Valeria; Arena, Giuseppe; Sciotto, Domenico; Sgarlata, Carmelo; Supramolecular Chemistry; vol. 25; 9-11; (2013); p. 615 – 625;,
Pyridine – Wikipedia,
Pyridine | C5H5N – PubChem