A class of aminocucurbituril and its preparation method
A technology of cucurbituril and amino group, applied in the field of cucurbituril and its preparation, can solve problems such as difficulty in surface modification, hindering application, unimproved water solubility and the like
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Embodiment 1
[0025] Embodiment 1: Preparation of aminocucurbit[6]urea
[0026] Dissolve 1.4g of CB[6] into 40ml of toluene, add the acid chloride solution, the molar ratio of CB[6] to the acid chloride solution is 1:12, place the solution in an environment protected by inert gas, and heat to reflux at 60-80°C for 12 After ~36h, the toluene was evaporated to obtain the imidazolium salt.
[0027] Add 12ml of ammonia organic solution (7mol / L) into imidazolium salt, heat and reflux at 60-80°C for 12-36h under the protection of inert gas, evaporate the solvent, add appropriate amount of deionized water, wash and dry , to obtain guanidine cucurbituril.
[0028] Disperse guanidine cucurbituril in a methanol medium, add a reducing agent (sodium borohydride or borane), the molar ratio of guanidine cucurbit[6]uril to reducing agent is 1:12, stir until the reaction is complete, remove methanol, and obtain Crude product of cucurbituril (2.26 g).
[0029] Add appropriate amount of dichloromethane an...
Embodiment 2
[0030] Embodiment 2: Preparation of aminocucurbit[7]urea
[0031] Dissolve 1.4g of CB[7] into 40ml of toluene solvent, add acid chloride solution, the molar ratio of CB[7] to acid chloride solution is 1:14, put the solution under the protection of inert gas, and heat to reflux at 60~80℃ After 12-36 hours, the toluene was distilled off to obtain the imidazolium salt.
[0032] Add 14ml of ammonia organic solution (7mol / L) into imidazolium salt, heat and reflux at 60-80°C for 12-36h under the protection of inert gas, evaporate the solvent, add appropriate amount of deionized water, wash and dry , to obtain guanidine cucurbituril.
[0033] Disperse guanidine cucurbituril in a methanol medium, add a reducing agent (sodium borohydride or borane), the molar ratio of guanidine cucurbit[7]uril to reducing agent is 1:14, stir until the reaction is complete, remove methanol, and obtain Crude product of cucurbituril (2.5 g).
[0034] Add appropriate amount of dichloromethane and water ...
Embodiment 3
[0035] Embodiment 3: Preparation of aminocucurbit[8]urea
[0036] Dissolve 1.4g of CB[8] into 40ml of toluene solvent, add acid chloride solution, the molar ratio of CB[8] to acid chloride solution is 1:16, put the solution under the protection of inert gas, and heat to reflux at 60~80℃ After 12-36 hours, the toluene was distilled off to obtain imidazolium salt as a solid.
[0037] Add 16ml of ammonia organic solution (7mol / L) into imidazolium salt, heat and reflux at 60-80°C for 12-36h under the protection of inert gas, evaporate the solvent, add appropriate amount of deionized water, wash and dry , to obtain solid guanidinium cucurbituril.
[0038] Disperse guanidine cucurbituril in a methanol medium, add a reducing agent (sodium borohydride or borane), the molar ratio of guanidine cucurbit[8]uril to reducing agent is 1:16, stir until the reaction is complete, remove methanol, and obtain Crude product of cucurbituril (2.2 g).
[0039] Add appropriate amount of dichloromet...
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