Related Products of 2533-69-9, In the next few decades, the world population will flourish. As the population grows rapidly and people all over the world use more and more resources, all industries must consider their environmental impact. 2533-69-9, name is Methyl 2,2,2-trichloroacetimidate belongs to chlorides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.
Step E4-[(4, 6- dicyclopropyl- 7-m ethyl- 1 H-benz imidazol-2-yl)carbon yl]-1-(trans-4- hydroxycyclohexyl)-2- piperazinone[00278] 4, 6-dicyclopropyl-3-methyl-1 , 2-benzenediamine (167 mg, 0.826 mmol) was dissolved in acetic acid (10 ml) before methyl 2,2,2-trichloromethylacetimidatate (0.146 ml, 1.16 mmol) was added drop-wise. The mixture was stirred at room temperature until the reaction was complete (~3 hours). The reaction was diluted with ethyl ether and then water added. The mixture was extracted 2 times with ethyl ether. The combined organic layers were washed with brine, dried over sodium sulfate, and concentrated. The residue was dissolved in acetonitrile (5 ml) before water (1.7 ml) was added. 1-(trans-4-hydroxycyclohexyl)-2-piperazinonehydrochloride (370 mg, 1.58 mmol) was added followed by drop-wise addition of potassium carbonate (4M) (0.789 ml, 3.15 mmol). The mixture was stirred for 1 hour. LC-MS showed none of the amide product, but the 2-carboxylic acid was observed. The reaction was concentrated and N,N-dimethylformamide (3 mL) added to the residue. N,N- diisopropylethylamine (0.551 ml, 3.15 mmol) was added followed by N-[(dimethylamino)(3H- [1 ,2,3]triazolot4,5-b]pyridin-3-yloxy)methylidene]-N-methylmethanaminium hexafluorophosphate (HATU) (360 mg, 0.946 mmol). The mixture was stirred for 2 hours and quenched with brine. The mixture was extracted 3 times with ethyl acetate. The combined organic layers were washed with brine, dried over sodium sulfate, and concentrated. The residue was purified by silica chromatography eluting with a gradient of 0% to 10% methanol in dichloromethane.Fractions were concentrated to leave the title compound (62 mg, 18%) as a white solid. LCMS: m/z 437 (M+1).
The synthetic route of Methyl 2,2,2-trichloroacetimidate has been constantly updated, and we look forward to future research findings.
Reference:
Patent; GLAXOSMITHKLINE LLC; BANKA, Anna; CATALANO, John G; FANG, Jing; PEAT, Andrew James; TAI, Vincent; TURNER, Elizabeth; WO2011/97491; (2011); A1;,
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