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. 2867-59-6, name is 3-Aminobutan-1-ol, molecular formula is C4H11NO, 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. Quality Control of 3-Aminobutan-1-ol
75 g of D-malic acid (0.56 mol) in 250 ml of anhydrous ethanol, stirred at room temperature, the system was dissolved, then added dropwiseA 50 g mixture of 3-amino-1-butanol (0.56 mol) in racemic mixture was added dropwise and warmed to 30-40C. The system was dissolved and 0.5 g of (S)-3-amino-1-butanol was added. D Malate salt as a seed crystal, and stirring during heat preservation, the solid precipitated after half an hour, continue to stir for 2 to 3 hours, slowly to room temperature, and continue to cool to 5 to 10 C for half an hour, suction filtration, to obtain an optical purity of 90.8 %ee.The D-malate salt of (S)-3-amino-1-butanol.The resulting (S)-3-amino-1-butanol D-malate with an optical purity of 90.8% ee was suspended in 200 ml of anhydrous ethanol, warmed to reflux, and the system was dissolved, slowly cooled, and the cooling process was solid. Gradually precipitated, cooled to room temperature, stirred for 1~2 hours, continued cooling to 5~10C, and kept stirring for 0.5 hour. Filtered to obtain an optical purity of 98.7%e.The D-malate salt of (S)-3-amino-1-butanol.The above-mentioned recrystallized D-malate salt of (S)-3-amino-1-butanol having an optical purity of 98.7% ee was suspended in 150 ml of anhydrous ethanol, and the temperature was raised to reflux. After the system was dissolved, the temperature was slowly lowered. The solids gradually precipitated, dropped to room temperature, incubated for 1 to 1.5 hours while stirring, and continued to cool down to 5 to 10C for half an hour, filtered by suction, and vacuum dried at 50C to a constant weight to give an optical purity of 99.4% ee.(S). D-malate salt of 3-amino-1-butanol.The above-mentioned recrystallized D-malate salt of (S)-3-amino-1-butanol having an optical purity of 99.4%ee was suspended in 120 ml of absolute ethanol, and the temperature was raised to reflux. After the system was dissolved, the temperature was gradually lowered. Solids gradually precipitated, dropped to room temperature, incubated for 1 to 1.5 hours while stirring, and continued to cool to 5 to 10C for half an hour, filtered, and vacuum dried at 50C to constant weight.50.4 g of D-malate salt with an optical purity of 99.9% ee.(S)-3-amino-1-butanol are obtained,Yield 40.3%.
With the rapid development of chemical substances, we look forward to future research findings about 2867-59-6.
Reference:
Patent; Shanghai Disainuo Pharmaceutical Co., Ltd.; Shanghai Disainuo Chemical Pharmaceutical Co., Ltd.; Yancheng Disainuo Pharmaceutical Co., Ltd.; Shanghai Chuangnuo Pharmaceutical Group Co., Ltd.; Li Jinliang; Zhao Nan; Wu Jun; (10 pag.)CN107793320; (2018); A;,
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