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. 1829-28-3, name is Ethyl 2-iodobenzoate, A new synthetic method of this compound is introduced below., Product Details of 1829-28-3
To a dried pressure tube was added o-phenylenediamine (0.3 g, 2.7 mmol), ethyl-2-iodobenzoate (1.5 g, 5.5 mmol) under nitrogen followed by ethylene glycol (6 mL), 10 mol % CuI (52 mg, 0.27 mmol) and K3PO4 tribasic (1.17 g, 5.5 mmol). Pressure tube was closed tightly and heated at 100 C for 4 h. After completion of the reaction (monitored by TLC) reaction mixture was cooled to room temperature and filtered over a pad of silica with CH2Cl2 to remove CuI and base residues. Then solvent was removed on rotary evaporator and the residue was purified on silica column chromatography using 25-30% EtOAc in hexane as solvent to give 1 Yield 50% (0.29 g). (0019) mp: 251-253 C; IR (upsilonmax):3320, 3025, 1603, 1579, 1471, 1394, 1157, 748 cm-1; 1H NMR (300 MHz, DMSO-d6): delta 8.63 (s, 1H, Amide NH), 6.60 (s, 1H, Amine NH), 6.46 (dd, J = 7.9, 1.4 Hz, 1H, ArH), 6.19-6.08 (m, 1H, ArH), 5.87-5.63 (m, 6H, ArH);13CNMR (75 MHz, DMSO): delta 168.1, 150.4, 140.0, 133.2, 131.9, 129.6, 124.6, 123.0, 122.7, 121.2, 120.9, 119.8, 119.0; HRMS (ESI) m/z calculated for [M+H]+ [C13H11N2O] 211.0866, found 211.0860.
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; Praveen Kumar, Chintakunta; Reddy, T. Srinivasa; Mainkar, Prathama S.; Bansal, Vipul; Shukla, Ravi; Chandrasekhar, Srivari; Huegel, Helmut M.; European Journal of Medicinal Chemistry; vol. 108; (2016); p. 674 – 686;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com