The synthetic route of 17347-61-4 has been constantly updated, and we look forward to future research findings.
With the rapid development and complex challenges of chemical substances, new drug synthesis pathways are usually the most effective.17347-61-4,2,2-Dimethylsuccinicanhydride,as a common compound, the synthetic route is as follows.
To a stirred solution of ((1R,3aS,5aR,5bR,7aR,9S,11aR,11bR,13aR,13bR)-9- hydroxy-5a,5b,8,8,11a-pentamethyl-1-(1-methylcyclopropyl)icosahydro-1H-cyclopenta[a]chrysen-3a-yl)(piperidin-1-yl)methanone (step 2, 0.16 g, 0.29 mmol, 1.0 eq) in ethyl acetate (2 ml) 2,2-dimethylsuccinicanhydride (0.114 g, 0.89 mmol, 3.0 eq) and DMAP (0.109 g, 0.89 mmol, 3.0 eq) were added sequentially then refluxed at about 100 ¡ãC for overnight. After completion of the reaction monitored by TLC, the reaction mixture was cooled to 0 ¡ãC, acidified with 1.0 N citric acid solution, organic layer was separated and extracted with ethyl acetate (2×30 ml). The combined organic layers were washed with water, brine solution, dried over Na2S04, filtered, evaporated and purified by silicagel column chromatography using 10percent EtOAc: hexane as eluent to afford the title compound (50 mg, 25percent yield) as an off-white solid. 1H NMR (300 MHz, DMSO-d6): delta 12.1 (s, 1H), 4.37 (dd, 1H, J= 10.8, 4.8 Hz), 3.52-3.37 (m, 4H), 2.82-2.72 (m, 1H), 2.45-2.39 (m, 2H), 2.12-2.04 (m, 1H), 1.98-1.85 (m, 2H), 1.70-1.50 (m, 8H), 1.48-1.28 (m, 12H), 1.28-1.22 (m, 5H), 1.18-1.15 (m, 6H), 1.12-1.07 (m, 1H), 0.95 (s, 3H), 0.90-0.73 (m, 16H), 0.37-0.27 (m, 2H), 0.23-0.13 (m, 2H); Mass: [M+H]+ 666.5 (70percent); HPLC: 98.6percent., 17347-61-4
The synthetic route of 17347-61-4 has been constantly updated, and we look forward to future research findings.
Reference£º
Patent; HETERO RESEARCH FOUNDATION; PANDURANGA ADULLA, Reddy; PARTHASARADHI REDDY, Bandi; MANOHAR SHARMA, Vedula; RATHNAKAR REDDY, Kura; PREM KUMAR, Mamnoor; BHASKAR REDDY, Kasireddy; NARSINGAM, Mogili; VENKATI, Mukkera; VL SUBRAHMANYAM, Lanka; MALLIKARJUN REDDY, Ravi; WO2013/160810; (2013); A2;,
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