Synthetic Route of 929-75-9, These common heterocyclic compound, 929-75-9, name is 1,11-Diamino-3,6,9-trioxaundecane, its traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route.
General procedure: A two-neck flask equipped with a magnetic stirrer and reflux condenser, flushed with dry argon, was charged with diazacrown derivative 4-9 (0.2-0.25 mmol), Pd(dba)2 (8-16 mol%), BINAP or DavePhos ligand (9-18 mol%), absolute dioxane (10-12 mL), the reaction mixture was stirred for several minutes, then the corresponding polyamine (0.2-0.25 mmol) and NaOt-Bu (0.6-0.75 mmol) were added, and the reaction mixture was stirred at reflux for 24 h. After cooling down to room temperature the residue was filtered off, washed with CH2Cl2 (5-10 mL), the combined organic fractions were evaporated in vacuo, the residue was dissolved in CH2Cl2 (10 mL), washed with distilled water (3 × 10 mL), dried over 4A molecular sieves, and the solvent was evaporated in vacuo. The solid residue was chromatographed on silica gel (40-60 mum) using a sequence of eluents: CH2Cl2, CH2Cl2-MeOH 100:1-3:1, CH2Cl2-MeOH-NH3(aq) 100:20:1-10:4:1.
The synthetic route of 929-75-9 has been constantly updated, and we look forward to future research findings.
Reference:
Article; Yakushev, Alexei A.; Chernichenko, Nataliya M.; Anokhin, Maxim V.; Averin, Alexei D.; Buryak, Alexei K.; Denat, Franck; Beletskaya, Irina P.; Molecules; vol. 19; 1; (2014); p. 940 – 965;,
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