Synthetic Route of 15103-48-7 , The common heterocyclic compound, 15103-48-7, name is Pyridine-2-sulfonic acid, molecular formula is C5H5NO3S, 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 dried Schlenck tube was charged with pyridine sulfonicacid (PySO3H,0.342 mmol) and KOtBu (0.342 mmol). Afteraddition of methanol, the reaction mixture was allowed to stirfor 30min then [RuCl2(p-cymene)]2 (0.1 g, 0.163 mmol)wasadded. The reaction mixture was stirred under nitrogen for 24h. The yellow suspension became a clear red solution withina few minutes. As the reaction progress, the solution becamecloudy then an orange-yellow solid appeared. The solid wascentrifuged and washed with diethyl ether (2 x 10 mL).The additional compound was obtained from the supernatantby subsequently drying, then dissolving the residuein dichloromethane followed by precipitation with hexane.Orange yellowsolid; yield: 106 mg (76%); Anal.Calcd. forC15H18ClNO3RuS:C41.96;H4.22;N3.26; S 7.45. Found:C41.86;H4.11;N3.58; S 7.24. FTIR (KBr, cm-1): 3051, 2974,1591, 1288, 1436; 1HNMR(CDCl3, delta): 8.76 (d, 1H, J= 5.1),8.01 (m, 1H), 7.88 (d, 1H, J=7.5), 7.57 (t, 1H), 5.78 (d, 1H, J=5.7), 5.69 (d, 1H, J= 5.7), 5.59 (d, 1H, J 6.0), 5.49 (d, 1H, J=6.0), 3.05 (m, 1H), 2.22 (s, 3H), 1.36 (t, 6H, J=7.2); 13CNMR(CDCl3, delta): 157.34, 153.57, 140.57, 127.84, 122.79, 103.97,97.65, 82.10, 81.92, 81.64, 80.54, 30.96, 22.91, 21.65, 18.39;ESI-MS: 394.0051 (M-Cl)+ calculated for C15H18NO3RuS,found 394.0026.
The synthetic route of 15103-48-7 has been constantly updated, and we look forward to future research findings.
Reference:
Article; Singh, Keisham S; Sawant, Sneha G; Kaminsky, Werner; Journal of Chemical Sciences; vol. 130; 9; (2018);,
Pyridine – Wikipedia,
Pyridine | C5H5N – PubChem