Reference of 150349-36-3,Some common heterocyclic compound, 150349-36-3, name is 3-(N-Boc-N-methylamino)propylamine, molecular formula is C9H20N2O2, 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.
Ethyl theophylline-7-acetate 2 (266mg, 1 mmol) was suspended in ethanol (1 mL) in a conical vial and N-methyl-N-Bocpropane-1,3-diamine (330 mg, 1.75 mmol) was added. The vial was sealed and heated up to 110OC for 2 h. After purification by column chromatography (DCM/MeOH/Et3N95:5:1 ? 80:20:1), Boc group was removed by stirring intermediate 3b in 4M HCl(5mL). Aliquote of crude reaction mixture (1/3 rd) was neutralized with concentrated NaHCO3 and inorganic salts were precipitated by addition of ethanol (100 mL). After filtration, the solvents were removed in vacuo and the residue was recrystallized from ethyl acetate (hot solution was filtered to eliminate residual traces of inorganic salts). Monomethylated compound 4 was obtained as white solid in 20% unoptimized yield (60mg, 0.2 mmol)
The synthetic route of 150349-36-3 has been constantly updated, and we look forward to future research findings.
Reference:
Article; Gibon, Julien; Kang, Min Su; Aliaga, Arturo; Sharif, Behrang; Rosa-Neto, Pedro; Seguela, Philippe; Barker, Philip A.; Kostikov, Alexey; Bioorganic and Medicinal Chemistry; vol. 24; 19; (2016); p. 4759 – 4765;,
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