Chiral polyalcohol and preparation thereof
A chiral and polyalcohol technology, applied in the field of chiral polyalcohol and its preparation, can solve problems such as poor thermal stability
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Embodiment 1
[0024] Pd(OAc) 2 (10.3mg, 0.046mmol), a mixture of P-PHOS (29.6mg, 0.046mmol) was added to a shlenk bottle, and CH 2 Cl 2 25ml, CH 3 OH 25ml and BF 3 ·Et 2 O 0.051mmol, stirred at room temperature for 1 hour, transferred into an autoclave, sealed the autoclave, replaced the air in the autoclave with propylene three times, cooled in an ice bath, filled with 35g of propylene, and then filled with CO to 4MPa. The temperature was raised to 50° C., and the reaction was carried out for 24 hours. Cool to room temperature, vent the unreacted gas, evaporate the solvent under reduced pressure, and dry in vacuo to obtain 3.3625 g of chiral polyketone, the conversion number is 717 g polymer / g Pd, and the molecular weight measured by gel permeation chromatography is 5.3×10 3 g / mol.
[0025] Dissolve the above polyketone (0.3g) in 30mlTHF, add 0.5gLiAlH 4 , at 60°C, stir magnetically for 12 hours, stop the reaction, let stand for 1 hour to precipitate the solid matter in the system,...
Embodiment 2
[0027] Dissolve the above polyketone (0.3g) in 30mlTHF, add 0.5gNaBH 4 , sonicate for 1 hour, add a small amount of distilled water dropwise to accelerate the reaction, stir at 50°C for 5 hours, stop the reaction, let the solid matter in the system settle for 1 hour, decant the supernatant, add 0.5ml of distilled water to the clear liquid to decompose the reaction The remaining solid reducing agent in the system was filtered, and the organic phase was anhydrous MgSO 4 After drying, the THF was distilled off under reduced pressure to obtain a transparent glassy polyalcohol with a yield of 97%. The IR spectrum shows that the polyketide carbonyl peak completely disappears at 3325cm -1 There is an obvious hydroxyl peak on the left and right, 1030cm -1 There is a C-O absorption peak, 13 In the C NMR spectrum, the 210ppm carbonyl carbon peak disappeared, and a strong α-carbon peak appeared at 61.64ppm. 1 The characteristic peak of hydroxyl hydrogen appeared at 4.93ppm in the H N...
Embodiment 3
[0029] Dissolve polyketone (0.3 g) in a shlenk flask with a small amount of THF, N 2 Inject 8ml of BH with a syringe under atmosphere 3 Slowly pour THF into the shlenk bottle, stir, react at 0°C for 1 hour, add 0.7ml distilled water to quench the reaction, and use anhydrous MgSO for the organic phase 4 dry. The inorganic substances in the system were removed by flash column chromatography to obtain a transparent glassy polyalcohol with a yield of 97%. The infrared spectrum shows that the carbonyl group is reduced to a hydroxyl group, 13 In the C NMR spectrum, the 210ppm carbonyl carbon peak disappeared, and the α-carbon peak appeared at 53.15ppm, 1 The characteristic peak of hydroxyl hydrogen appeared at 5.23ppm in the H NMR spectrum.
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