A new synthetic route of 929-75-9

Statistics shows that 929-75-9 is playing an increasingly important role. we look forward to future research findings about 1,11-Diamino-3,6,9-trioxaundecane.

929-75-9, name is 1,11-Diamino-3,6,9-trioxaundecane, belongs to ethers-buliding-blocks compound, is considered to be a conventional heterocyclic compound, which is widely used in drug synthesis. The chemical synthesis route is as follows. 929-75-9

Example 174 (3S)-3-(2-benzyl-3-chloro-7-oxo-2,4,5,7-tetrahydro-6H-pyrazolo[3,4-c]pyridin-6-yl)-N-(13-((3S)-3-(2-benzyl-3-chloro-7-oxo-2,4,5,7-tetrahydro-6H-pyrazolo[3,4-c]pyridin-6-yl)-5-methyl-4-oxo-2,3,4,5-tetrahydro-1,5-benzoxazepin-8-yl)-13-oxo-3,6,9-trioxa-12-azatridec-1-yl)-5-methyl-4-oxo-2,3,4,5-tetrahydro-1,5-benzoxazepine-8-carboxamide To a mixture of (S)-2,4,6-trichlorophenyl 3-(2-benzyl-3-chloro-7-oxo-4,5-dihydro-2H-pyrazolo[3,4-c]pyridin-6(7H)-yl)-5-methyl-4-oxo-2,3,4,5-tetrahydrobenzo[b][1,4]oxazepine-8-carboxylate (50 mg) and tetrahydrofuran (2 mL) were added 2,2′-((oxybis(ethane-2,1-diyl))bis(oxy))diethanamine (7.28 mg), triethylamine (7.66 mg) and 4-dimethylaminopyridine (0.46 mg) at room temperature, and the mixture was stirred at 50C for 2 hr. The reaction mixture was diluted with ethyl acetate, washed with 0.1 M hydrochloric acid, saturated aqueous sodium hydrogencarbonate solution and saturated brine, and dried over anhydrous sodium sulfate, and the solvent was evaporated under reduced pressure. The residue was purified by silica gel column chromatography (ethyl acetate/methanol) to give the title compound (27.1 mg). 1H NMR (300 MHz, CDCl3) delta2.66 (2H, dt, J = 15.9, 4.7 Hz), 3.03 (2H, ddd, J = 15.5, 10.4, 5.1 Hz), 3.29-3.39 (5H, m), 3.45-3.81 (17H, m), 4.15-4.27 (2H, m), 4.29-4.43 (2H, m), 4.52-4.71 (2H, m), 5.38 (4H, s), 5.85 (2H, dd, J = 11.5, 8.1 Hz), 7.11 (2H, brs), 7.18-7.35 (10H, m), 7.62-7.76 (4H, m).

Statistics shows that 929-75-9 is playing an increasingly important role. we look forward to future research findings about 1,11-Diamino-3,6,9-trioxaundecane.

Reference:
Patent; Takeda Pharmaceutical Company Limited; YOGO, Takatoshi; YOSHIKAWA, Masato; SAITOH, Morihisa; KATOH, Taisuke; SEKI, Tomohiro; NAKADA, Yoshihisa; (148 pag.)EP3366684; (2018); A1;,
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