Hydroxy fatty acid oligomer and application in regulating calcium ion concentration in cell
A cell and oligomerization technology, applied in the direction of drug combination, metabolic disease, cardiovascular system disease, etc., can solve the problem of high price
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Embodiment 1
[0054] The preparation of embodiment 1 3-hydroxybutyric acid oligomer (OHB)
[0055] Accurately weigh 3 g of poly-3-hydroxybutyrate-4-hydroxybutyrate (P3HB4HB), add 200 ml of dichloromethane, and reflux at 90°C. After the PHB is completely dissolved, add 0.3 g of p-toluenesulfonic acid and 0.5 g of water, continue the reflux reaction for 1 hour, and then add 0.5 g of water. After 2 hours, the reaction was terminated, filtered, precipitated with cold methanol, filtered, extracted by a Soxhlet extractor for 12 hours, and then dried under vacuum at 50°C for 48 hours for later use. The number-average molecular weight (number-average molecular weight or Mn) detected by gel permeation chromatography (GPC, Waters1515) is 2000, and the nuclear magnetic resonance spectrum (NMR, Bruker 400) analysis product does not contain cytotoxic substances such as ethylenic bonds.
Embodiment 2
[0056] Example 2 Preparation of oligomeric 3-hydroxybutyrate methyl ester (OHB-CH3)
[0057] Dissolve 1 g of PHB in 50 mL of chloroform, heat to reflux at 60°C for 2 hours to fully dissolve, add dropwise 50 mL of concentrated sulfuric acid methanol solution (10% v / v), and heat to reflux at 90°C for 2 hours. Add 50mL of methanol pre-cooled at 4°C, let stand for 1h, centrifuge the mixed solution at 8000rpm, 4°C for 20min, discard the supernatant, add methanol to resuspend. Repeat the above steps twice, dry under vacuum at 50°C for 48 hours for later use, and obtain OHB-OCH containing 3 Solid white powder. Gel permeation chromatography (GPC, Waters 1515) detected that the Mn was 2000, and nuclear magnetic resonance spectroscopy (NMR, Bruker 400) analyzed that the product did not contain cytotoxic substances such as ethylenic bonds.
Embodiment 3
[0058] Example 3 Oligomeric 3-hydroxybutyrate-4-hydroxybutyrate methyl ester (O3HB4HB-CH 3 ) preparation
[0059] Dissolve 1g of P3HB4HB in 50mL of chloroform, heat to reflux at 60°C for 2h to fully dissolve, add 50mL concentrated sulfuric acid methanol solution (10% v / v) dropwise, and heat to reflux at 90°C for 2h. Add 50mL of methanol pre-cooled at 4°C, let stand for 1h, centrifuge the mixed solution at 8000rpm, 4°C for 20min, discard the supernatant, add methanol to resuspend. Repeat the above steps twice, dry under vacuum at 50°C for 48 hours for later use, and obtain OHB-OCH containing 3 Solid white powder. The Mn detected by gel permeation chromatography (GPC, Waters 1515) is 2100, and the nuclear magnetic resonance spectrum (NMR, Bruker 400) analyzes that the product does not contain cytotoxic substances such as ethylenic bonds.
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