R-1-aminoindan preparation method
A technology of aminoindane and mandelic acid, which is applied in the purification/separation of amino compounds, organic chemistry, etc., can solve the problems of expensive resolution catalyst, troublesome post-processing, low selectivity, etc., and achieve good effect, reasonable selection, and resolution The effect of simple method
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Embodiment 1
[0007] (1)
[0008] In a 1000ml round bottom flask, add 18.2G (0.12mol) L-mandelic acid to a mixed solution of methanol (200ml) and water (100ml), heat to 50°C, add 13.3G (0.1mol) of 1-aminoindane ), reflux reaction for 1.5 hours, cooled to room temperature, and filtered to obtain the crude product of L-mandelate salt of R-1-aminoindane. The resulting salt was added to a mixture of methanol (100ml) and water (50ml) for recrystallization to obtain 11.5g of L-mandelate salt of R-1-aminoindane.
[0009] (2)
[0010] Dissolve 11.5g of L-mandelate salt of R-1-aminoindane obtained in the previous step in 200ml of water, add dropwise 40% sodium hydroxide solution to adjust the pH value to 12, and extract with dichloromethane (100ml, 50ml, 50ml) Three times, the dichloromethane layers were combined, washed with water (50ml) and saturated brine (50ml) once each, dried over anhydrous sodium sulfate, filtered, and concentrated to obtain 4.8g of R-1-aminoindane with a yield of 36%, ee ...
Embodiment 2
[0014] (1)
[0015] In a 1000ml round bottom flask, add 22.8G (0.15mol) of L-mandelic acid into a mixed solution of ethanol (200ml) and water (200ml), heat to 50°C, add 13.3G (0.1mol) of 1-aminoindane ), reflux reaction for 1.0 hour, cooled to room temperature, and filtered to obtain the crude product of L-mandelate salt of R-1-aminoindane. The resulting salt was added to a mixture of ethanol (110ml) and water (40ml) for recrystallization to obtain 10.6g of L-mandelate salt of R-1-aminoindane.
[0016] (2)
[0017] Dissolve 10.6 g of L-mandelate salt of R-1-aminoindane obtained in the previous step in 300 ml of water, add ammonia water dropwise to adjust the pH value to 13, extract 3 times with ethyl acetate (100 ml, 50 ml, 50 ml), dichloro The methane layers were combined, washed once with water (50ml) and saturated brine (50ml), dried over anhydrous sodium sulfate, filtered, and concentrated to obtain 4.0g of R-1-aminoindane with a yield of 30% and an ee value of 99.4%.
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