Enoxolone derivative, preparation method and uses
A technology of glycyrrhetinic acid and medicines, applied in the field of glycyrrhetinic acid derivatives, preparation and application, which can solve the problems of limiting the clinical application of glycyrrhetinic acid, the inability to prepare injections, and vascular irritation, so as to reduce irritation and vasospasm , Solve the solubility and improve the effect of safety
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Embodiment 1
[0031] Example 1: Preparation of glycyrrhetinic acid arginine
[0032] Add 2.35 g (0.005 mol) of glycyrrhetinic acid, 0.87 g (0.005 mol) of L-arginine, and 440 mL of 90% ethanol (V / V) to the reaction flask, stir and react for 2 hours, and evaporate the solvent under reduced pressure. Add 20 mL of ethyl acetate to the residue, grind to obtain a pale yellow precipitate, filter, and dry under reduced pressure to obtain 3.0 g of a pale yellow solid with a yield of 93%. Glycyrrhetinic acid was used as a reference substance for content determination, and the product content was 99.7%.
[0033] Glycyrrhetinic acid arginine shows the following physical and chemical properties:
[0034] Properties: light yellow powder mp: 183~186℃.
[0035] ESI-MS m / z: 644([M-H] + ).
[0036] Elemental analysis% calculated value (actual value): C 67.05 (67.48), H9.38 (9.27), N8.69 (8.81).
[0037] Molecular formula: (C 36 H 60 N 4 O 4 )
[0038] UVλ max nm: 258IR (KBr, v max , Cm -1 ): 3172(-NH 2 , -OH), 1647 ...
Embodiment 2
[0040] Example 2: Preparation of Glycyrrhetinic Acid Arginine
[0041] Add 2.35 g (0.005 mol) of glycyrrhetinic acid, 0.87 g (0.005 mol) of L-arginine, and 440 mL of 85% ethanol (V / V) to the reaction flask, stir and react for 2 hours, and evaporate the solvent under reduced pressure. Add 20 mL of ethyl acetate to the residue, grind to obtain a light yellow precipitate, filter, and dry under reduced pressure to obtain 3.1 g of a light yellow solid with a yield of 96%. Glycyrrhetinic acid was used as a reference substance for content determination, and the product content was 99.6%.
Embodiment 3
[0042] Example 3: Preparation of Glycyrrhetinic Acid Arginine Injection
[0043] Glycyrrhetinic acid arginine salt (prepared according to Example 1) 5g
[0044] Propylene glycol 150g
[0045] Sodium citrate 10g
[0046] Add water for injection to 1000ml
[0047] Weigh the prescription amount of glycyrrhetinic acid arginine salt, dissolve it in propylene glycol under heating, add sodium citrate and water for injection, adjust the pH to 9.0 with 5% NaOH, add 0.1% activated carbon and stir for 30 minutes, filter, and dispense into ampoules Medium, 1ml per tube, sterilize at 115°C for 30 minutes, it is ready.
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Abstract
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