In the next few decades, the world population will flourish. As the population grows rapidly and people all over the world use more and more resources, all industries must consider their environmental impact. 25245-27-6, name is 1-Iodo-3,5-dimethoxybenzene belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. Formula: C8H9IO2
To a solution of 5-iodo-1,3-dimethoxybenzene (8, 20.98 g, 79.5 mmol) in dry DMF (75 mL), cooled to 0 C, was dropwise added POCl3 (42.64 g, 278.1 mmol). The reaction mixture was gradually warmed to room temperature and subsequently heated to 85 C. After stirring for 5 h at 75 C, the reaction mixture was poured into iced water (400 mL) and extracted with EtOAc (3*300 mL). The combined organic layer was washed with satd aq NaHCO3 (300 mL), dried over Na2SO4, and concentrated under reduced pressure. Recrystallization from hexanes/EtOAc (3/1) yielded benzaldehyde 9 (18.43 g, 79%) as a yellow solid; Rf 0.3 (hexanes/EtOAc=3/1); 1H NMR (200 MHz, CDCl3) delta 10.12 (s, 1H), 7.11 (d, J=2.3 Hz, 1H), 6.47 (d, J=2.2 Hz, 1H), 3.88 (s, 3H), 3.85 (s, 3H); 13C NMR (50 MHz, CDCl3) delta 190.6 (d, 1C), 164.6 (s, 1C), 163.3 (s, 1C), 119.2 (d, 1C), 118.3 (s, 1C), 99.1 (d, 1C), 98.6 (s, 1C), 56.0 (q, 1C), 55.9 (q, 1C); HRMS m/z calcd for [M+Na]+ 314.9489, found 314.9500; Anal. Calcd for C9H9IO3: C, 37.01; H, 3.11; found: C, 37.22; H, 3.14.
The synthetic route of 25245-27-6 has been constantly updated, and we look forward to future research findings.
Reference:
Article; Mikula, Hannes; Skrinjar, Philipp; Sohr, Barbara; Ellmer, Doris; Hametner, Christian; Froehlich, Johannes; Tetrahedron; vol. 69; 48; (2013); p. 10322 – 10330;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com