Some common heterocyclic compound, 36076-26-3, name is Diethyl 2,2-(1,4-phenylene)diacetate, molecular formula is C14H18O4, 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. COA of Formula: C14H18O4
1-1 Ethyl 2-nitrobenzene-1,4-diacetate A solution of ethyl benzene-1,4-diacetate (CAS Reg. No. 36076-26-3) (14.0 g; 55.937 mmol) prepared in accordance with JP-A 57-183740 in conc. sulfuric acid (28 ml) was cooled with ethanol/dry ice, and 90% nitric acid (4.0 g; 57.134 mmol) was added dropwise thereto at -5 to 10 C. After 10 min., the reaction solution was added dropwise to a solution of ethyl acetate (140 ml) in ice-water (140 ml). Then, the organic layer was separated and washed with water, a saturated aqueous sodium bicarbonate and brine, followed by adding anhydrous magnesium sulfate and activated charcoal thereto. After filtering, the solvent was removed, to give the title compound (yield: 16.16 g, 54.726 mmol, 97.8%). m.p.: 50-51 C.; 1H-NMR(400 MHz, CDCl3) delta (ppm); 1.27 (3H, t, J=7.1 Hz) 1.28 (3H, t, J=7.1 Hz), 3.70 (2H, s), 4.00 (2H, s), 4.17 (2H, q, J=7.1 Hz), 4.18 (2H, q, J=7.1 Hz), 7.32 (1H,d, J=7.9 Hz), 7.53 (1H, dd, J=7.9, 1.5 Hz), 8.05 (1H, d, J=1.5 Hz).
These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 36076-26-3, its application will become more common.
Reference:
Patent; Eisai Co., Ltd.; US6573384; (2003); B1;,
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