20781-20-8, In the chemical reaction process, reaction time, type of solvent, can easily affect the result of the reaction, thereby determining the yield and properties of the reaction product. An updated downstream synthesis route of 20781-20-8 as follows.
To a solution of(2R,6R,I 1R)-tert-butyl 6,1 i-dimethyh8(trifiuoromethyl)sulfonyl)oxy)-i ,2,5,6-tetrahydro-2,6-methanobenzo[diazocine3(4H)carboxyiate (5.32 g, 11.8 mmoi) in degassed dimethyl sulfone (50 mL), wasadded Nhydroxysuccinimide (233 g, 23.7 rnmoi), palladium acetate (265 nig, 118 mmol), triethylamine (3.3 mL, 23,7 mmoi) and 4,5-bis(diphenylphosphino)95- dimethyixanthene (683 mg, 1.1 8 mrnoi). The reaction mixture was heated with carbon monoxide (latm) at 70C overnight. The reaction mixture was cooled toambient temperature and 2,4-dimethoxybenzylamine (2.17 mg. 13.0 rnmol) added. The mixture was stirred for 2 hours diluted with ethyl acetate (800 rnL), and filtered tiu?ough cehte. The organic solution was washed twice with water (800 inL), hrine (300 mL), and dried (MgSO4). Filtration and removal of the solvent under reduced pressure gave crude material that was purified by silica chromatography(EtOAc(i):heptanes(l)) to give (2R,6R.l 1R)-tert-butyi 8-((2,4- dimethoxyhenzyl)carhamoyi)6, Ii dimethyl- I ,2,5,6..tetrahydro-2,6- methanohenzo[dazocine-3(4i-I)-carhoxyla1e (4.0 g, 68% yield); L.C/MS(M+H) = 495,3,
According to the analysis of related databases, (2,4-Dimethoxyphenyl)methanamine, the application of this compound in the production field has become more and more popular.
Reference:
Patent; ALKERMES PHARMA IRELAND LIMTED; DEAVER, Dan; BLUMBERG, Laura, Cook; EYERMAN, David; WYNN, Thomas; WO2014/190271; (2014); A2;,
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