120737-78-2, tert-Butyl 2-methylpiperazine-1-carboxylate is a piperazines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated
To a solution of 7-(3,4-dimethoxyphenyl)-5-methyl-4-oxo-4,5-dihydrothieno[3,2-c]pyridine-2- carbaldehyde (for a preparation see Intermediate 25, 100 mg, 0.304 mmol) in DCM (5 mL) was added acetic acid (0.026 mL, 0.455 mmol) and ierf-butyl 2-methylpiperazine-1 -carboxylate (0.073 mL, 0.364 mmol) and the reaction mixture was stirred under nitrogen at room temperature for one hour. Sodium triacetoxyborohydride (322 mg, 1.518 mmol) was then added and the reaction was refluxed under nitrogen overnight. The reaction mixture was allowed to cool to room temperature and was then hydrolyzed with a saturated aqueous solution of sodium bicarbonate (20 mL). The layers were separated and the aqueous phase was extracted with DCM (3 x 10 mL). The combined organic layers were washed with a saturated aqueous solution of sodium chloride solution (approx. 20 mL), dried over magnesium sulphate, filtered and concentrated under vacuum to give a light brown residue. The residue was purified by chromatography on silica gel eluting with 0 to 5% MeOH in DCM. The appropriate fractions were combined to give an impure light brown residue. The product was therefore loaded onto a 2g SCX column and was flushed with MeOH (3 column volumes). The product was eluted in 2.0M ammonia in MeOH (3 column volumes) and concentrated to give ferf-butyl 4-((7-(3,4-dimethoxyphenyl)-5-methyl-4-oxo-4,5-dihydrothieno[3,2-c]pyridin-2- yl)methyl)-2-methylpiperazine-1-carboxylate (1 10 mg, 71 % yield) as a yellow oil. LCMS (2 min, Formic Acid): Rt = 0.90 min, MH+ = 514, 120737-78-2
120737-78-2 tert-Butyl 2-methylpiperazine-1-carboxylate 15087784, apiperazines compound, is more and more widely used in various fields.
Reference£º
Patent; GLAXOSMITHKLINE LLC; AMANS, Dominique; BAMBOROUGH, Paul; BIT, Rino, Antonio; BROWN, John, Alexander; CAMPBELL, Matthew; LINDON, Matthew, John; SHIPLEY, Tracy, Jane; THEODOULOU, Natalie, Hope; WELLAWAY, Christopher, Roland; WESTAWAY, Susan, Marie; WO2014/78257; (2014); A1;,
Piperazine – Wikipedia
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