Reference of 65896-11-9, 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 65896-11-9 as follows.
To a solution of 2-(l-(((9Eta-fluoren-9-yl)methoxy)carbonyl)-4-(ter£- butoxycarbonyl)piperazin-2-yl)acetic acid (5 g, 10.72 mmol) in dichloromethane (100 mL) with Lambda/,Lambda/-dimethylformamide (2 drops) was added oxalyl dichloride (3.4 g, 26.8 mmol). The reaction mixture was stirred at room temperature for 1 hour, then concentrated. Tetrahydrofuran (100 mL) was added to the concentrate followed by the slow addition of a solution containing 2-bromo-6-fluoroanaline (3 g, 16 mmol) and diisopropylethylamine (9 mL) in tetrahydrofuran (20 mL). The solution was stirred at room temperature for 2 hours before the addition of piperazine (2.77 g, 32.2 mmol) after which the solution was stirred for 15 hours. The reaction mixture was concentrated onto silica gel and purified via flash chromatography (0-100 % ethyl acetate/hexane, then 0-10 % methanol/dichloromethane) to afford the title compound. 1H NMR (300 MHz, DMSO-J6) delta ppm 7.47 – 7.65 (m, 1 H) 7.21 – 7.46 (m, 2 H) 3.55 – 4.05 (m, 2 H) 2.67 – 3.14 (m, 3 H) 2.49 – 2.67 (m, 2 H) 2.26 – 2.46 (m, 2 H) 1.39 (s, 9 H); MS (APCI+) m/z 418.2 (M+H)+.
According to the analysis of related databases, 65896-11-9, the application of this compound in the production field has become more and more popular.
Reference:
Patent; ABBOTT LABORATORIES; ABBOTT GMBH &; CO. KG; WANG, Ying; BREWER, Jason, T.; AKRITOPOULOU-ZANZE, Irini; DJURIC, Stevan, W.; POHLKI, Frauke; BRAJE, Wilfried; RELO, Ana-Lucia; WO2010/124042; (2010); A2;,
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bromide – Wiktionary