A kind of preparation method of ester
A technology of glyceryl behenate and behenic acid, which is applied in the preparation of pharmaceutical excipients and the field of glyceryl behenate, can solve the problem that glyceryl behenate is difficult to meet the quality requirements of pharmaceutical excipients, and achieve cost Low, easy to operate and control, the effect of low reaction temperature
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Embodiment 1
[0025] In the reactor, add 136.40g behenic acid, 44.60g glycerin, 4.60g p-toluenesulfonic acid monohydrate, 200mL mixed solvent of cyclohexane and n-heptane (volume ratio 1:4), add The same mixed solvent is 32mL, stirred, heated to reflux; the water separator is divided into water, refluxed for 11 hours to 12 hours, and the reaction is stopped; the reaction mixture is cooled to 60°C, added to 400mL of ice water, stirred for 1 hour, and a solid is precipitated , filtered; the obtained solid was vacuum dried at 40°C for 8 hours to 10 hours; the obtained solid was mixed with 1000mL isopropyl ether, stirred at 20°C to 30°C for 0.5 hour to 1 hour, filtered, and the solid was vacuum dried at 35°C for 20 hours to 24 hours ; Obtain white product 150.35g, HPLC detects, and ester content meets the requirements.
Embodiment 2
[0027] In the reactor, add 136.40g behenic acid, 44.60g glycerol, 4.60g p-toluenesulfonic acid monohydrate, add 225mL of mixed solvent of cyclohexane and n-heptane (volume ratio 1:4), in the water separator Add 30mL of the same mixed solvent, stir, and heat to reflux; the water separator divides the water, reflux for 12-13 hours, and stop the reaction; cool the mixed solution to 60°C, add 450mL of cold acetone and water mixed solution ( Volume ratio 1:4), stirred for 1 hour, filtered; the obtained solid was vacuum-dried at 40°C for 8 hours; the obtained solid was mixed with 900mL isopropyl ether, stirred for 1 hour at 25°C-30°C, filtered, and the solid was vacuum-dried at 35°C for 24 hours ; Obtain 150.08g of white product, and HPLC detects that the ester content meets the requirements.
Embodiment 3
[0029] In the reactor, add 136.40g behenic acid, 50.00g glycerol, 3.90g p-toluenesulfonic acid monohydrate, add 180mL of mixed solvent of cyclohexane and n-heptane (volume ratio 1:5), in the water separator Add 25mL of the same mixed solvent, stir, and heat to reflux; divide the water with the water separator, reflux for 13-14 hours, and stop the reaction; cool the mixed solution to 60°C, add it to 400mL of cold water, and stir for 1-1.5 hours , filtered; the obtained solid was vacuum-dried at 40°C for 8 hours to 10 hours; the obtained solid was mixed with 1100mL isopropyl ether, stirred at 20°C for 45 minutes, filtered, and the solid was dried at 35°C for 24 hours; 149.78g of white product was obtained, which was detected by HPLC. The content meets the requirements.
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Abstract
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