Application of 6276-54-6, These common heterocyclic compound, 6276-54-6, name is 3-Chloropropan-1-amine hydrochloride, 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.
3-chloropropylamine-HCL (5 g, 38.46 mmole, 1.0 equiv) was dissolved in 20 mL dry DCM under inert atmosphere. DIPEA (5.47g , 42.31 mmole, 1.1 equiv) was added via syringe at room temperature to the stirring mixture. When the solution was clear and all reagents solubilized, the reaction mixture was cooled to 00C. Under inert atmosphere, boc-anhydride (8.4 g, 38.49 mmole, 1.1 equiv) was dissolved in 5 mL dry DCM. This solution was added slowly to the stirring solution of 3-chloropropylamine-HCL at 00C. After addition, the solution was allowed to warm up to R.T. and mix for 5 hrs while monitoring for completion by TLC and LC/MS. Upon completion, 25 mL of H2O was added to the reaction at ambient atmosphere while mixing. The mixture was then diluted, transferred to a seperatory funnel, and the water layer extracted into DCM (3 x 20 mL). The organic layer was dried over Na2SO4, filtered, and evaporated to dryness to afford a crude powder. The product was purified by Hex: EtOAc silica chromatography using a CombiFlash purification system. Product eluted at 2 : 1 Hex: EtOAc and collected fractions were evaporated to dryness to afford S1-1 as a white powder (MW: 193.67 g/mol, 6.08 g, 82% yield).1H NMR (400 MHz, CDCl3): 3.58 (t, J = 6.4 Hz, 2H), 3.27 (m, 2H), 1.96 (m, 2H), 1.43 (s, 9H).
Statistics shows that 3-Chloropropan-1-amine hydrochloride is playing an increasingly important role. we look forward to future research findings about 6276-54-6.
Reference:
Patent; THE REGENTS OF THE UNIVERSITY OF CALIFORNIA; SHOKAT, Kevan, M.; GENTILE, Daniel; MOSS, Steven; (380 pag.)WO2018/112420; (2018); A1;,
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