Electric Literature of 112970-44-2, A common heterocyclic compound, 112970-44-2, name is 2-Bromo-3-methoxyaniline, molecular formula is C7H8BrNO, 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-bromo-3-methoxyaniline B4 (0.79 g; 3.9 MMOL) in MEOH (7.6 mL) was added dimethyl acetylene dicarboxylate A3 (0.53 mL; 4.3 MMOL) dropwise at 0 C (caution: reaction is exothermic.). The solution was heated overnight at reflux and worked-up. The MEOH was evaporated and the crude product dried under high vacuum to afford a red gum, purified by flash column chromatography (1: 30 ultra pure silica gel, 230-400 mesh, 40-60 mm, 60 angstroms; 4: 1 hexane/EtOAc) to afford adduct B5 (86 %; 1.16 g) as a pale yellow solid. MS 344. 0 (MH) + ; Homogeneity by HPLC (TFA) 220 nm: 72%.
The synthetic route of 112970-44-2 has been constantly updated, and we look forward to future research findings.
Reference:
Patent; BOEHRINGER INGELHEIM INTERNATIONAL GMBH; BOEHRINGER INGELHEIM PHARMA GMBH & CO KG; WO2004/103996; (2004); A1;,
Ether – Wikipedia,
Ether | (C2H5)2O – PubChem