Alanine substituted calix[4]arene bonded silica stationary phase and preparation method and application thereof
A technology for bonding silica gel and alanine, which is applied in the field of separation science, can solve the problems of limited performance of bonded phases and few types of calixarene bonded phases, and achieves good identification and separation performance, high bonding amount and stable performance. Effect
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[0031] 2. Preparation of γ-aminopropyltrimethoxy bonded silica gel
[0032] Take 5.0 mL of γ-aminopropyltrimethoxysilane in a 500 mL three-neck round bottom flask, add 200 mL of freshly distilled anhydrous toluene, add 10.0 g of activated silica gel under magnetic stirring, and add 0.4 mL of triethylamine (anhydrous ), install the return line and CaCl 2 Dry the tube and reflux for 24 h under nitrogen protection. Stop the reaction, filter with a G5 sand core funnel, wash with toluene, acetone, double-distilled water, and acetone in sequence, and dry in vacuum at 80°C for 8 h to obtain γ-aminopropyltrimethoxy bonded silica gel.
[0033] 3. Preparation of 25,27-bis(L-alanine methyl ester-N-carbonylmethoxy)-26,28-dihydroxy-p-tert-butylcalix[4]arene bonded stationary phase
[0034]Weigh 3.0 g of 25,27-bis(L-alanine methyl ester-N-carbonylmethoxy)-26,28-dihydroxy-p-tert-butylcalix[4]arene in a 100 mL three-neck round bottom flask , add 50 mL freshly steamed anhydrous toluene, und...
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