Synthetic Route of 82560-12-1, 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. 82560-12-1 name is 3-Amino-5-tert-butylpyrazole, 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.
Intermediate A14: 3-ferf-Butyl-1 -(4-methylthiophen-2-yl)-1 H-pyrazol-5-amine.; Intermediate A14; To a sol ution of 2-iodo-4-methylthiophene (WO 2008/121666) (1 .00 g, 4.50 mmol) in anhydrous toluene (15.0 mL) was added 3-ie f-butyl-1 /-/-pyrazol-5-amine (683 mg, 4.91 mmol) followed by (1 R,2R)-/V1,/V2-dimethylcyclohexane-1 ,2-diamine (140 mu, 0.89 mmol) and potassium carbonate (1.30 g, 9.37 mmol). The mixture was purged with N2, copper(l) iodide (42 mg, 0.22 mmol) was added and the reaction mixture was heated at reflux under N2 for 16 hr during which time most of the solvent was lost. The resulting mixture was partitioned between ethyl acetate (150 mL) and water (150 mL) and the organic layer was separated and extracted with aq. citric acid solution (10% w/v, 150 mL) followed by brine (50 mL), and then dried and evaporated in vacuo. The residue was purified by flash column chromatography (Si02, 120 g, DCM, isocratic elution) to afford the title compound, Intermediate A14, as a brown solid (340 mg, 32%); R’ 1.94 min (Method 2); m/z 236 (M+H)+ (ES+).
At the same time, in my other blogs, there are other synthetic methods of this type of compound, 3-Amino-5-tert-butylpyrazole, and friends who are interested can also refer to it.
Reference:
Patent; RESPIVERT LIMITED; MURRAY, Peter, John; ONIONS, Stuart, Thomas; WILLIAMS, Jonathan, Gareth; JOLY, Kevin; WO2011/158044; (2011); A2;,
Pyrazole – Wikipedia,
Pyrazoles – an overview | ScienceDirect Topics