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Stage #1: (1R,2S)-2-aminocyclohexan-1-ol With (-)-dibenzoyl-L-tartaric acid monohydrate In ethanol at 20 - 25℃; for 2.66667h; Reflux;
Stage #2: With hydrogenchloride In water monomer
8 Example 8
In the reaction flask, intermediate 3 (11.5 g, 0.1 mol) was mixed with 45 mL of ethanol, and completely dissolved under stirring. The temperature was controlled at 20-25°C, and L-DBTA-H2O (18.8g, 0.05mol) and 90mL of ethanol mixed solution were added dropwise, and the dropwise addition was completed in 40 minutes, and then the temperature was heated and refluxed for 2 hours; the reaction system was lowered to 0°C by gradient cooling. , a solid was precipitated in the process, and the diastereoisomeric salt was obtained by filtration, which was recrystallized with 90 mL of ethanol, and the white solid salt was obtained by filtration. The white solid salt was added with 3N aqueous hydrochloric acid solution to pH=2-3, extracted with ethyl acetate twice (for L-DBTA recovery), the water layer was distilled under reduced pressure, and toluene was added with water during the finishing process until the solid crude product was obtained , after beating with ethanol and drying, 5.8 g of off-white solid (1R,2S)-2-aminocyclohexanol hydrochloride was obtained.
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