Method for separating tropicamide raceme
A technology of tropicamide and racemate, which is applied in the field of medicinal chemistry to achieve the effect of precise medication
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Embodiment 1
[0057] Add 10g of tropicamide racemate (35mmol) into 35ml of (R)-(+)-1-phenylethanol, stir to dissolve, add dropwise 10ml of 1g of (S)-(+)-ammonium lactate and 1.6 g (18.3mmol) (S)-(+)-lactic acid prepared as a methanol solution, after the dropwise addition, the temperature was raised to 65°C, and the methanol was distilled off. Let stand, cool down to 18°C for crystallization, and filter.
[0058] Dissolve the filter cake in 20ml of water, add 15ml of chloroform, adjust the pH to 9-10 with 3N sodium hydroxide solution under stirring, separate the layers, wash the organic phase twice with 10ml of water, and recover the chloroform by distillation. Dry under reduced pressure at 60°C for 2 hours to obtain 4.1 g of pure (S)-(-)-tropicamide, [α]=-54.3°.
[0059] 30ml of water and 30ml of chloroform were added to the filtrate, the pH was adjusted to 1-2 with 2N sulfuric acid, the layers were separated, and the aqueous phase was washed twice with 10ml of chloroform respectively. ...
Embodiment 2
[0061] Add 10g of tropicamide racemate (35mmol) into 30ml of (R)-(+)-1-phenylethanol, stir to dissolve, add dropwise 10ml of 1g of (S)-(+)-ammonium lactate and 1.6 g (18.3mmol) (S)-(+)-lactic acid prepared as a methanol solution, after the dropwise addition, the temperature was raised to 65°C, and the methanol was distilled off. Let stand, cool down to 20°C for crystallization, and filter.
[0062] Dissolve the filter cake in 20ml of water, add 15ml of chloroform, adjust the pH to 9-10 with 3N sodium hydroxide solution under stirring, separate the layers, wash the organic phase twice with 10ml of water, recover the chloroform by distillation, and dry under reduced pressure at 60°C In 2 hours, 4.5 g of pure (S)-(-)-tropicamide was obtained, [α]=-49.7°.
[0063] Add 30ml of water and 25ml of chloroform to the filtrate, adjust the pH to 1-2 with 2N sulfuric acid, separate the layers, and wash the aqueous phase twice with 10ml of chloroform respectively. Add 25ml of chloroform t...
Embodiment 3
[0065] Add 10g of tropicamide racemate (35mmol) into 40ml of (R)-(+)-1-phenylethanol, stir to dissolve, add dropwise 10ml of 1g of (S)-(+)-ammonium lactate and 1.6 g (18.3mmol) (S)-(+)-lactic acid prepared as a methanol solution, after the dropwise addition, the temperature was raised to 65°C, and the methanol was distilled off. Let stand, cool down to 17°C for crystallization, and filter.
[0066] Dissolve the filter cake in 20ml of water, add 15ml of chloroform, adjust the pH to 9-10 with 3N sodium hydroxide solution under stirring, separate the layers, wash the organic phase twice with 10ml of water, recover the chloroform by distillation, and dry under reduced pressure at 60°C In 2 hours, 3.9 g of pure (S)-(-)-tropicamide was obtained, [α]=-56.3°.
[0067] Add 30ml of water and 30ml of chloroform to the filtrate, adjust the pH to 1-2 with 2N sulfuric acid, separate the layers, and wash the aqueous phase twice with 10ml of chloroform respectively. Add 25ml of chloroform t...
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