Method for separating and purifying crown ether stereoisomer
A technology for separation and purification of stereoisomers, applied in the direction of organic chemistry, etc., can solve the problems of increasing the complexity of the system, cumbersome separation and elution process, low yield, etc., achieving excellent extraction ability and selectivity, and simple process flow. Ease of implementation, avoids the effect of complexity
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Embodiment 1
[0022] Di-tert-butylcyclohexyl cyclohexa-18-crown-6 isomer mixture obtained by catalytic hydrogenation (see the attached figure 1 ) 20g was dissolved in 100mL ethylene glycol dimethyl ether, kept stirring, and heated to 70°C. Then 8 g of strontium chloride hexahydrate was added, and the mixture was stirred and refluxed for 1 hour. The strontium salt was filtered out while it was hot, and the filtrate was cooled and allowed to stand to precipitate white complex crystals. The crystals were collected, dried and dissolved in 100 mL of dichloromethane. During the dissolution process of the complex, a large amount of strontium chloride salt will precipitate out. After separating the precipitate, the filtrate was washed three times with 300 mL of aqueous nitric acid at pH 3. The organic phase was rotary evaporated to remove dichloromethane, and dried in vacuo to obtain a white solid with a yield of 69.8%. Determined by gas chromatography (attached figure 2 ), the white solid is...
Embodiment 2
[0024] Dissolve 10 g of di-tert-butylcyclohexa-18-crown-6 isomer mixture obtained by catalytic hydrogenation in 60 mL of ethylene glycol dimethyl ether, keep stirring, and heat to 70°C. 5 g of strontium chloride hexahydrate was added thereto, and the mixture was stirred and refluxed for 1 hour. The strontium salt was filtered out while it was hot, and the filtrate was cooled and allowed to stand to precipitate white complex crystals. The crystals were collected, dried and dissolved in 70 mL of chloroform. During the dissolution process of the complex, a large amount of strontium chloride salt will precipitate out. After separation of the precipitate, the filtrate was washed three times with 210 mL of aqueous nitric acid at pH 3. The organic phase was rotary evaporated to remove chloroform, and dried in vacuo to obtain a white solid, which was di-tert-butylcyclohexyl-18-crown-6 on Sr 2+ It has high-efficiency extraction ability and selective isomer components, and the yield ...
Embodiment 3
[0026] Dissolve 10 g of di-tert-butylcyclohexyl-18-crown-6 isomer mixture in 60 mL of ethylene glycol dimethyl ether, keep stirring, and heat to 70°C. To the solution was added 5 g of strontium chloride hexahydrate and refluxed for 1 hour. Filtrate the undissolved strontium salt while it is hot, and the filtrate is cooled and allowed to stand to precipitate white complex crystals. The crystals were collected, dried and dissolved in 60 mL of carbon tetrachloride. During the dissolution process of the complex, a large amount of strontium chloride salt will precipitate out. After separating the precipitate, the filtrate was washed twice with 100 mL of aqueous nitric acid at pH 2. The organic phase was rotary evaporated to remove carbon tetrachloride, and dried in vacuo to obtain a white solid, which was di-tert-butylcyclohexyl-18-crown-6 to Sr 2+ It has high-efficiency extraction ability and selective isomer components, and the yield is 67.5%.
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