Synthetic Route of 13330-96-6, As we all know, there are many different methods for the synthesis of a compound, and people can choose the synthesis method that suits their own laboratory according to the actual situation. 13330-96-6, name is 4-(Dimethylamino)butan-1-ol, molecular formula is C6H15NO, The compound is widely used in many fields, so it is necessary to find a new synthetic route. The downstream synthesis method of this compound is introduced below.
To a mixture of sodium hydride (72%, 232 mg, 7.0 mmol) and tetrahydrofuran (20 ml) was added 4-(dimethylamino)-1-butanol (0.82 g, 7.0 mmol) at 0C (external temperature), and the reaction mixture was stirred at 45C for 20 minutes. Then, the reaction mixture was cooled at 0C (external temperature). To the reaction mixture was added dropwise a mixture of tributyl-iodomethyl-tin (2.0 g, 4.6 mmol) and N,N-dimethylformamide (20ml) at the same temperature. Then, the reaction mixture was stirred at 45C for 30 minutes. The reaction mixture was brought to room temperature, water and ethyl acetate were added to the reaction mixture, and the organic layer was separated. The organic layer was washed with water and an aqueous saturated sodium chloride solution, and the solvent was distilled off under reduced pressure. The residue was purified by silica gel column chromatography (heptane: ethyl acetate=20:1, NH silica gel) to obtain the title compound (1.4 g, 3.3 mmol, 70%). 1H-NMR Spectrum (CDCl3) delta (ppm) : 0.81-0.97 (15H, m), 1.26-1.35(6H, m), 1.47-1.55(10H, m), 2.21(6H, s), 2.24-2.28(2H, m), 3.30-3.33(2H, m), 3.71(2H, t, J=6.8Hz).
According to the analysis of related databases, 13330-96-6, the application of this compound in the production field has become more and more popular.
Reference:
Patent; Eisai R&D Management Co., Ltd.; EP1867650; (2007); A1;,
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