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. 7425-53-8, name is Ethyl 4-iodobutanoate, A new synthetic method of this compound is introduced below., Product Details of 7425-53-8
In a round bottom flask, compound 16 (5.0 g, 22.12 mmol) was dissolved in dry THF (50 mL) over an ice bath and sodium hydride (NaH, 1.25 g, 52.08 mmol) was added to the solution. After 20 min. stirring, ethyl 4-iodobutyrate (10.74 g, 44.24 mmol) was added to the reaction mixture. The solution was kept over ice-bath for 15 min., and then transferred to room temperature. The progress of reaction was monitored by TLC. After completion of reaction, the reaction mixture was quenched with saturated solution of NH4Cl and worked up with ethyl-acetate and washed with water. The organic layer was separated, dried over anhydrous sodium sulphate (Na2SO4) and concentrated. The crude product was then chromatographed over a column of silicagel (100-200 mesh) eluting with the ethyl acetate-hexane (2:98) to afford compound 21a as white solid. Yield: 70%; mp: 50-51C; Rf: 0.60 (30% Ethyl acetate-Hexane); IR (KBr, numax/cm-1): 2957, 1729, 1673, 1599, 1261, 1026, 830, 741; 1H NMR (CDCl3, 500 MHz, delta ppm): 1.21 (t, J = 7.0 Hz, 3H, CH3), 1.25-1.65 (m, 2H, CH2), 1.83 (d, J = 5.0 Hz, 1H, CH2), 2.16 (t, J = 5.5 Hz, 1H, CH2), 2.27-2.32 (m, 2H, CH2), 3.81 (s, 3H. OCH3). 4.08 (q, J = 7.0 Hz, 2H, OCH2), 4.49 (t, J = 7.0 Hz, 1H, CH), 6.84-6.87 (m, 2H, ArH), 7.17-7.20 (m, 1H, ArH), 7.26-7.30 (m, 4H, ArH), 7.93-7.96 (m, 2H, ArH); 13C NMR (CDCl3, 125 MHz, delta ppm): 14.2, 23.1, 33.4, 34.2, 53.1, 55.4, 60.2, 113.7 (2xC), 127.0, 128.1 (2xC), 128.9 (2xC), 129.7, 130.9 (2xC), 139.7, 163.3, 173.4, 198.0; EIMS (C21H24O4): m/z = 341.2 [M+H]+.
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; Bawankule, Dnyaneshwar U.; Gupta, Atul; Imran Ahamad, Mohd.; John, Aijaz A; Khan, Feroz; Luqman, Suaib; Prakash, Ravi; Singh, Divya; Wani, Zahoor; Yadav, Deepika; Bioorganic and medicinal chemistry letters; (2020);,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com