At the same time, in my other blogs, there are other synthetic methods of this type of compound, 4-Bromo-1-iodo-2-nitrobenzene, and friends who are interested can also refer to it.
Related Products of 112671-42-8, As we all know, there are many different methods for the synthesis of a compound, and people can choose the synthesis method that suits their own laboratory according to the actual situation. 112671-42-8 name is 4-Bromo-1-iodo-2-nitrobenzene, This compound is widely used in many fields, so it is necessary to find a new synthetic route. The downstream synthesis method of this compound is introduced below.
To a mixture of 4-bromo-1-iodo-2-nitrobenzene (21.1g, 0.064mol) (described in Synthesis, (2008), (13), 2039-2044), cyclopropyl boronic acid (7.2g, 0.083mol), tricyclohexyl phosphine (1.7g, 0.0064mol) and potassium phosphate (50.Og, 0.24mol) is added toluene (255ml) and distilled water (23ml). The stirred mixture is degassed then flushed with nitriogen (cycle repeated x 3), followed by addition of palladium (II) acetate (0.7Og, 0.0032mol) and heating at 100C overnight. After cooling to room temperature the mixture is quenched with distilled water and extracted with ethyl acetate (x 3). All organics fractions are combined, washed with distilled water then brine, and dried over magnesium sulfate. Concentration in vacuo affords an approximate 6:4 mixture of 5- bromo-2-cyclopropylnitrobenzene and 4-bromo-1-iodo-2-nitrobenzene (11.9g) as a brown oil. To this crude mixture is then added additional cyclopropyl boronic acid (1.8g, 0.021 mol), tricyclohexylphosphine (0.43g, 0.0016mol), palladium acetate (0.18g, O.OOOdeltamol), potassium phosphate (12.5g, O.Odeltamol), toluene (65ml) and water (6ml). After heating at 100C overnight the suspension is allowed to cool to room temperature and the mixture is quenched with distilled water and extracted with ethyl acetate (x 3). All organics fractions are combined, washed with distilled water then brine, and dried over magnesium sulfate. Concentration in vacuo affords a crude product which is purified by flash column chromatography on silica gel to give a mixture of 5-bromo-2- cyclopropylnitrobenzene, 3-bromo-nitrobenzene and 2,5-dicyclopropyl-nitrobenzene which is used in the next step without further purification
At the same time, in my other blogs, there are other synthetic methods of this type of compound, 4-Bromo-1-iodo-2-nitrobenzene, and friends who are interested can also refer to it.
Reference:
Patent; SYNGENTA LIMITED; WHITTINGHAM, William, Guy; MATHEWS, Christopher, John; WAILES, Jeffrey, Steven; JEANMART, Stephane, Andre, Marie; ROBINSON, Louisa; WO2010/81894; (2010); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com