A triptycene oxygen-containing linear diol functional material, its preparation and application
A functional material, triptycene technology, applied in the field of gas chromatography to achieve high-efficiency separation, stable structure, and low raw material cost
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Embodiment 1
[0042] The specific preparation steps of triptycene oxygen-containing linear diol compound TP-HEO are as follows:
[0043] (1) Anthracene and p-benzoquinone were dissolved in xylene at a molar ratio of 1:1.2, and refluxed at 140°C for 5h, then cooled at 0°C for 12h, filtered to obtain a solid, and then washed with boiling water, and placed in Recrystallize in xylene, then wash with xylene and petroleum ether in turn to obtain triptycene-p-benzoquinone;
[0044] (2) Dissolve triptycene-p-benzoquinone in glacial acetic acid, heat and reflux for 1 hour, slowly add HBr in an equimolar amount to triptycene-p-benzoquinone to form a precipitate, continue to react for 0.5 hours, and cool in an ice bath , filter and collect the solid product, that is, triptycene-p-benzodihydroquinone (TP-2OH) is obtained;
[0045] The characterization results of the H NMR spectrum of TP-2OH: 1 H NMR (400MHz, acetone) δ7.83(s,2H),7.46–7.37(m,4H),7.02–6.93(m,4H),6.39(s,2H),5.93(s,2H);
[0046] (3) in ...
Embodiment 2
[0052] The specific preparation steps of triptycene oxygen-containing linear diol compound TP-PEG400 are as follows:
[0053] (1) in N 2 Under protection, PEG400 (polyethylene glycol, molecular weight 400) and triethylamine were dissolved in anhydrous dichloromethane at a molar ratio of 4:2.5, stirred at 0°C, and 0.01 times the molar amount of triethylamine was added 4-Dimethylaminopyridine, and dropwise add p-toluenesulfonyl chloride 0.25 times the molar amount of PEG400, react for 2h, cool and collect the crude product, wash the crude product with hydrochloric acid, distilled water, and saturated brine successively, and then use sodium sulfate Dry, then wash with eluent (V 二氯甲烷 :V 甲醇 =9:1) separation and purification on a silica gel column to obtain p-toluenesulfonate;
[0054] (2) TP-2OH prepared in step (2) of Example 1, p-toluenesulfonyl ester prepared in step (1) of this example, and potassium carbonate were refluxed in acetonitrile for 24 hours in a molar ratio of 1:...
Embodiment 3
[0058] The specific preparation steps of triptycene oxygen-containing linear diol compound TP-PCL2000 are as follows:
[0059] (1) in N 2 Under protection, dissolve PCL2000 (polycaprolactone diol, molecular weight 2000) and triethylamine in anhydrous dichloromethane at a molar ratio of 2:2.5, stir at 0°C, and add 0.5 times the amount of PCL2000 moles dropwise. A certain amount of p-toluenesulfonyl chloride, reacted for 24h, extracted with deionized water, dichloromethane, 1mol / L sodium hydroxide solution successively, dried the organic phase with anhydrous sodium sulfate, and washed with eluent (V 乙酸乙酯 :V 石油醚 =1:1) separation and purification on a silica gel column to obtain PCL-OTS (p-toluenesulfonate);
[0060] The characterization results of PCL-OTS proton NMR spectrum: 1 H NMR (400MHz, chloroform) δ7.71-7.73(m,2H),7.27-7.29(m,2H),3.93-4.04(t,36H),2.38(s,3H),1.97-2.26(t ,36H),1.58(s,70H),1.19-1.35(t,35H);
[0061] (2) in N 2 Under protection, the TP-2OH prepared in st...
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