Porous polymer compound, method of separating compound to be separated, single crystals, method of producing sample for crystal structure analysis, method of determining molecular structure of compound to be analyzed, and method of determining absolute configuration of chiral compound
a technology compounds, applied in the field of porous polymer compounds, can solve the problem of not so many porous polymer compounds reported to be usable for such purposes
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production example 1
Synthesis of Ligand 1
[0175]
[0176]Penta-O-acetyl-D-mannose (1.95 g, 5.00 mmol) and hydroquinone (275 mg, 2.50 mmol) were dissolved in 20 ml of dichloromethane in a 50 ml eggplant flask, and to the resulting solution was added boron trifluoride-diethylether complex (0.63 mL), and the resulting mixture was stirred for 24 hours at 20° C. The reaction solution was washed with 5% sodium hydrogen carbonate solution (40 mL) and water (20 mL), dried with anhydrous sodium sulfate, and the solvent was distilled with a rotary evaporator.
[0177]Crude product was purified with a recycle type size exclusion chromatography, and deca-O-acetylated product of ligand 1 was obtained [yield (amount) 1.0 g, yield (rate) 52%].
[0178]Then, deca-O-acetylated product of ligand 1 (200 mg, 0.26 mmol) and sodium methoxide (1.5 mg, 0.026 mmol) were dissolved in 10 ml of methanol, and the solution was stirred for 1 hour at 20° C. The resulting solution was neutralized by being passed through an ion-exchange resin, D...
production example 2
Synthesis of Ligand 2
[0185]
[0186]Penta-O-acetyl-D-mannose (3.96 g, 10.15 mmol) and 1,3,5-tri(4-hydroxyphenyl) benzene (1.2 g, 3.36 mmol) were dissolved in 120 ml of dichloromethane in a 200 ml eggplant flask, and boron trifluoride-diethylether complex (16.8 mL) and 510 mg of triethylamine were added to the resulting solution, and the resulting mixture was stirred for 38 hours at 60° C. The reaction solution was washed with 5% sodium hydrogen carbonate solution (40 mL) and water (20 mL), dried with anhydrous sodium sulfate, and the solvent was distilled with a rotary evaporator.
[0187]Crude product was purified with a recycle type size exclusion chromatography, and pentadeca-O-acetylated product of ligand 2 was obtained [yield (amount) 3.0 g, yield (rate) 67%].
[0188]Then, pentadeca-O-acetylated product of ligand 2 (800 mg, 0.595 mmol) and sodium methoxide (6.7 mg, 0.12 mmol) were dissolved in 100 ml of methanol, and the solution was stirred for 3 hours at 20° C. The resulting solution...
production example 3
Synthesis of Ligand 3
[0194]
[0195]Ligand 3 was synthesized according to a method disclosed in the following literature.[0196]Xu, Z.; Lee, S.; Lobkovsky, E. B.; Kiang, Y.-H., Journal of the American Chemical Society, 2002, Vol. 124, pp. 121-135
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