Synthetic Route of 95970-05-1, A common heterocyclic compound, 95970-05-1, name is 2,6-Dibromo-4-methoxyaniline, molecular formula is C7H7Br2NO, its 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.
To a solution of 2,6-dibromo-4-methoxyphenylamine (3 g, 10.67 mmol, 1 eq) in 10 ml of toluene cooled at 0° C. are added 6.6 ml of concentrated sulfuric acid and 17.5 ml of H3PO2 50percent (15 eq). To the reaction mixture, sodium nitrite (1.47 mg, 21.35 mmol, 2 eq) is added, and all is stirred at 0° C. for 4.5 h. After neutralization with a sodium hydroxide solution, extraction with diethyl ether is performed. The organic phase is dried over magnesium sulfate, filtered and evaporated to dryness on a rotary evaporator. Purification of the raw product was not necessary (yield 96percent, 2.7 g). C7H6Br2O; MW 264/266/268; 1H-NMR (CDCl3): delta 7.23-7.22 (m, 1H), 6.97 (s, 1H), 6.96 (s, 1H), 3.75 (s, 3H); 13C-NMR: delta 160.8, 126.4, 123.1, 116.5, 55.7; IR: 2925, 1599, 1569, 1464 1/cm
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:
Patent; Hartmann, Rolf; Frotscher, Martin; Oberwinkler, Sandrine; Ziegler, Erika; Messinger, Josef; Thole, Heinrich-Hubert; US2010/204234; (2010); A1;,
Ether – Wikipedia,
Ether | (C2H5)2O – PubChem