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Synthesis method of polyethyleneglycol-12-hydroxystearate

A technology of hydroxystearate and hydroxystearic acid, applied in the field of synthesis of polyethylene glycol-12-hydroxystearate, can solve the problems of difficult control, narrow molecular weight distribution, severe and the like

Active Publication Date: 2014-08-13
HUNAN ER KANG PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The method has high selectivity, narrow molecular weight distribution, and mild reaction, which solves the problem of reaction site selectivity in ethoxylation reaction, and the problem that ethoxylation reaction is too violent, difficult to control, and wide molecular weight distribution.

Method used

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  • Synthesis method of polyethyleneglycol-12-hydroxystearate
  • Synthesis method of polyethyleneglycol-12-hydroxystearate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0044] Example 1 Preparation of selective hydroxyl protecting agent tris (benzhydryl) phosphate

[0045] raw material:

[0046] Benzophenone hydrazone (CAS No.: 5350-57-2), purchased from Bailingwei, with a purity of 95%;

[0047] Iodobenzenediacetic acid (CAS No.: 3240-34-4), purchased from Bailingwei, with a purity of 98%;

[0048] 85% phosphoric acid, dichloromethane, sodium chloride, and ethyl acetate are commercially available analytical reagents.

[0049] The above reagents were used directly without any pretreatment.

[0050] step:

[0051] (a) Put 58.8g (0.3mol) of benzophenone hydrazone and 11.5g (0.1mol) of 85% phosphoric acid into 500ml of dichloromethane solvent, add 3.2g (0.01mol) of iodobenzenediacetic acid as a catalyst, at 40 ℃ reflux reaction for 4h;

[0052] (b) After the reaction, wash with saturated NaCl solution, 100ml each time until the washing solution is neutral, combine the organic layers, dry with anhydrous sodium sulfate for 2 hours, evaporate ...

Embodiment 2

[0054] Example 2 Preparation of Ethoxylation Reaction Composite Catalyst

[0055] Put 15.8g of magnesium acetate solid and 17.4g of potassium hydroxide solid into the mortar, grind for 15 minutes and mix them evenly, then add 17.1g of barium sulfate powder in batches under the grinding state, and continue grinding after adding the barium hydroxide solid 30 min, and then vacuum-dried at 70° C. for 2 h to obtain a catalyst.

Embodiment 3

[0056] Embodiment 3 Preparation of polyethylene glycol-12-hydroxystearate

[0057] raw material:

[0058] 12-Hydroxystearic acid (CAS No.: 106-14-9), purchased from Qingdao Tongkai Castor Chemical Co., Ltd., premium product.

[0059] Ethylene oxide and other inorganic and organic chemical reagents are commercially available industrial grade or analytically pure products.

[0060] The operation method is as follows:

[0061] First, it is the pretreatment step of hydroxystearic acid, that is, the step of protecting the hydroxyl group of 12-hydroxystearic acid.

[0062] 1) Take 30.0g (0.1mol) 12-hydroxystearic acid, add appropriate amount of CH 2 Cl 2 The solvent is made into a solution, and a selective hydroxyl protecting agent (Ph 2 CHO) 3 PO 61.4g (0.103mol), and 0.57g (0.005mol) trifluoroacetic acid catalyst, heated to reflux for 2-4h;

[0063] 2) Wash the reaction solution with purified water and saturated NaCl solution until the washing solution is neutral, combine t...

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Abstract

The invention discloses a synthesis method of polyethyleneglycol-12-hydroxystearate, which comprises the following steps: 1) hydroxystearic acid pretreatment; 2) ethoxylation with epoxyethane; and 3) deprotection, and separation and purification of the product. The method can be used for preparing the polyethyleneglycol-12-hydroxystearate which can be used in medicines.

Description

technical field [0001] The invention discloses a method for synthesizing polyethylene glycol-12-hydroxystearate, which belongs to the field of chemical industry. Background technique [0002] Polyethylene glycol-12-hydroxystearate, its structural formula is as follows: [0003] [0004] It can be used as a solubilizer and emulsifier in pharmaceutical preparations. An ideal drug should have good biosolubility and bioavailability when entering the body. However, among the drugs produced according to the prior art, 40% of the candidate drugs have solubility problems. To prepare suitable preparations for insoluble drugs, the problem of low solubility must first be solved. More than one-third of the workload in the drug development process is devoted to improving the solubility and bioavailability of poorly soluble drugs. Therefore, increasing the solubility or dissolution rate of poorly soluble drugs is one of the toughest challenges facing pharmaceutical scientists today....

Claims

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Application Information

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IPC IPC(8): C08G65/28
Inventor 帅放文王向峰章家伟
Owner HUNAN ER KANG PHARMA
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