Reference of 112-26-5,Some common heterocyclic compound, 112-26-5, name is 1,2-Bis(2-chloroethoxy)ethane, molecular formula is C6H12Cl2O2, 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.
The synthesis of precursor P4 was realized by a Williamsonether procedure. To a solution of 1.50 g (9.92 mmol) of 4-(acetylamino)phenol (1) in anhydrous DMF (30 mL) andinert N2 atmosphere, were added 10.0 equivalents of anhydrousK2CO3, whereupon the mixture was stirred over30 minutes at 120C. Subsequently were added 755 mul(4.90 mmol) of 1,2-bis(2-chloroethoxy)ethane (P2) and 1.0equivalent of KI. The mixture was maintained with stirringover a twelve-hour period at 120C. Finally, the mixture wasfiltered in order to remove the salt, then the solvent wasevaporated in vacuum and acetone was added. A precipitatewas obtained, which was filtered, washed with acetoneand then with water and vacuumdried to give a whitesolid. Yield: 1.83 g (90%). Melting point: 160-161C. IR (KBr,nu, cm-1): 3306, 1659, 1594, 1530, 1243. 1H NMR (400 MHz,DMSO-d6, delta, ppm, J, Hz): 9.84 (s, 2H, H-8), 7.45 (d, J= 9.0, 4H,H-6), 6.84 (d, J =9.0, 4H,H-5), 4.02 (t, J = 4.7, 4H, H-3), 3.71 (t,J = 4.7, 4H, H-2), 3.60 (s, 4H, H-1), 1.99 (s, 6H, H-10). 13CNMR(101 MHz, DMSO-d6, delta, ppm): 167.7 (C-9), 154.2 (C-4), 132.6(C-7), 120.5 (C-6), 114.4 (C-5), 69.9 (C-1), 69.0 (C-2), 67.2 (C-3),23.8 (C-10). ESI-MS: m/z (positive ion mode) 416.9 [M + H]+(28.55%), 454.9 [M + K]+ (82.30%), 871.9 [2M+K]+ (23.92%).Elem. Anal. Calcd for C22H28N2O6.H2O: C, 60.82; H, 6.96; N,6.45; O, 25.78. Found: C, 60.9; H, 6.37; N, 6.23.
The synthetic route of 112-26-5 has been constantly updated, and we look forward to future research findings.
Reference:
Article; Gomez-Vega, Jancarlo; Moreno-Corral, Ramon Alfonso; Santacruz Ortega, Hisila; Corona-Martinez, David Octavio; Hoepfl, Herbert; Sotelo-Mundo, Rogerio R.; Ochoa-Teran, Adrian; Escobar-Picos, Raymundo Enrique; Ramirez-Ramirez, Jose Zeferino; Juarez-Sanchez, Octavio; Lara, Karen Ochoa; Supramolecular Chemistry; vol. 31; 5; (2019); p. 322 – 335;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics