Some common heterocyclic compound, 5460-32-2, name is 4-Iodo-1,2-dimethoxybenzene, molecular formula is C8H9IO2, 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. Formula: C8H9IO2
Step 1: A mixture of I (117.0 g, 590 mmol), 4-iodo-1,2-dimethoxybenzene (85.0 g, 590 mmol), Pd(OAc)2 (13.2 g, 59 mmol) and tri(o-tolyl)phosphine (36.0 g, 118 mmol) in triethylamine (3 L) was heated at 90¡ã C. for 12 h. The mixture was cooled to room temperature and diluted with ethyl acetate (3 L). The organic phase was washed with brine, dried (MgSO4), and concentrated in vacuo to dryness. The crude product was purified by silica gel chromatography (0 to 40percent ethyl acetate/hexanes) to provide (1a) as a brown oil (87.0 g, 73percent based on the recovered starting material). 1H NMR (300 MHz, CDCl3): delta 6.85 (s, 2H), 6.79 (s, 1H), 6.64 (s, 1H), 3.98-3.93 (m, 4H), 3.88 (s, 3H), 3.86 (s, 3H), 2.10-2.00 (m, 4H), 1.81 (s, 3H), 1.68 (d, J=12.9 Hz, 4H), 1.17 (s, 1H).
These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 5460-32-2, its application will become more common.
Reference:
Patent; Sequoia Sciences, Inc.; Williams, Russell B.; (17 pag.)US2017/73324; (2017); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com