Electric Literature of 7681-82-5, These common heterocyclic compound, 7681-82-5, name is Sodium iodide, 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.
To a solution of [3]- (50 mg, 0.081 mmol) in acetonitrile (2 mL), chloramine-T (37 mg, 0.129 mmol),sodium iodide (15 mg, 0.097 mmol) and acetic acid (130 L) were added. The reaction mixture wasallowed to stir at room temperature for 10 h. For the workup, 20 mL of water were added and extractedwith ethyl acetate (3 x 15 mL), the organic layers were combined and washed with brine solution beforedrying over anhydrous sodium sulphate. The solvent was evaporated and the crude was purifiedusing column chromatography (silica gel, 10% MeOH in dichloromethane) to yield [5]- as a yellowsolid (25 mg, 41.6%). 1H-NMR (methanol-d4) delta 4.27 [Cc-H, 2H, s], 4.13 [Cc-H, 2H, s], 3.37 [CH2O, 2 H,t], 2.85 [CH2-S, 2 H, t], 2.31 [CH3, 3 H, s], 1.55 [CH2-CH2-O, 2 H, m], 1.45 [CH2-CH2S, 2 H, m], 1.36[CH2-CH2CH2O, 2 H, m]; 11B-NMR (methanol-d4) delta 21.47 [1B, s], 0.42[2B, d, 1J(B-H) = 145.4], 4.39[1B, s], 5.71 [4B, d, 1J(B-H) = 140.0], 7.27 [4B, d, 1J(B-H) = 152.8], 18.07 [2B, d, 1J(B-H) = 152.4],20.04 [2B, d, 1J(B-H) = 161.3], 23.45 [1B, d, 1J(B-H) = 161.3], 27.37 [1B, d, 1J(B-H) = 170.4]; 13C-NMR(CDCl3) delta 191.05, 70.24, 58.99, 56.52, 34.78, 33.10, 32.97, 32.52, 29.24. LCMS (ESI) Experimental [M]- m/z = 606.6 (theoretical [M]- m/z = 607.6).
Statistics shows that Sodium iodide is playing an increasingly important role. we look forward to future research findings about 7681-82-5.
Reference:
Article; Pulagam, Krishna R.; Gona, Kiran B.; Gomez-Vallejo, Vanessa; Meijer, Jan; Zilberfain, Carolin; Estrela-Lopis, Irina; Baz, Zurine; Cossio, Unai; Llop, Jordi; Molecules; vol. 24; 19; (2019);,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com