35736-52-8, name is 2,4-Dibromo-5-methoxyaniline, belongs to ethers-buliding-blocks compound, is considered to be a conventional heterocyclic compound, which is widely used in drug synthesis. The chemical synthesis route is as follows. Quality Control of 2,4-Dibromo-5-methoxyaniline
2,4-Dibromo-5-methoxyaniline (930 mg, 3.31 mmol) and paraformaldehyde (160 mg, 5.30 mmol) were dissolved in trifluoroacetic acid (30 mL). The reaction mixture was stirred under an argon atmosphere in dark for 48 h. The reaction mixture was then basified with a solution of concentrated ammonia (30 mL) in water (30 mL). A saturated sodium hydrogen carbonate solution (100 mL) was added and the aqueous mixture was extracted into dichloromethane (3×50 mL). The combined organic layers were washed with brine (100 mL), dried over anhydrous sodium sulfate, filtered and evaporated to dryness. The crude material was chromatographed (silica, dichloromethane) to afford (+/-)-18 (450 mg, 53%) as a pale off-white solid: mp 181-182 C; Rf (CH2Cl2) 0.22; IR (neat) numax 2938, 2895, 2848, 1604, 1486, 1442, 1420, 1247, 1195, 1082 cm-1; 1H NMR (400 MHz, CDCl3) delta 3.74 (s, 3H, OCH3), 3.84 (s, 3H, OCH3), 4.15-4.33 (m, 4H, CH2), 4.47 (d, J 17.0 Hz, 1H, CH2), 4.52 (d, J 17.0 Hz, 1H, CH2), 6.66 (s, 1H, ArH), 7.09 (s, 1H, ArH), 7.61 (s, 1H, ArH); 13C NMR (100 MHz, CDCl3) delta 54.1, 55.3, 56.2, 60.2, 66.5, 107.1, 108.3, 111.5, 114.7, 120.8, 125.5, 131.0, 134.6, 145.4, 147.4, 153.5, 155.0; Anal. Calcd for C17H15Br3N2O2.0.1 CH2Cl2: C 38.93; H 2.90; N 5.31. Found: C 38.85; H 2.73; N 5.06%.
The synthetic route of 35736-52-8 has been constantly updated, and we look forward to future research findings.
Reference:
Article; Malik, Qasim M.; Ijaz, Sadia; Craig, Donald C.; Try, Andrew C.; Tetrahedron; vol. 67; 32; (2011); p. 5798 – 5805;,
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