Method for producing polyethylene glycol-glycerol derivative and intermediate thereof
A technology of glycerin derivatives and polyethylene glycol, which is applied in the production of bulk chemicals, etc., can solve the problems of high cost and cumbersome preparation process of PEG-Gly, and achieve the effects of reducing process cost, easy acquisition and high yield
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[0027] In a typical embodiment of the present application, a method for preparing a polyethylene glycol-glycerin derivative intermediate is provided, the preparation method comprising: esterifying raw materials including polyethylene glycol and sulfonyl chloride resin reaction to obtain a first product system comprising a polyethylene glycol-glycerol derivative intermediate, and at least one end group of polyethylene glycol is a hydroxyl group, wherein the above-mentioned sulfonyl chloride resin is a polystyrene resin containing a sulfonyl chloride group , the structural formula of sulfonyl chloride resin is expressed as .
[0028] The present application utilizes the resin polymer solid-phase properties of the sulfonyl chloride resin, and a solid-phase synthesis method can be used to prepare a product system comprising a polyethylene glycol-glycerin derivative intermediate. Specifically, the sulfonyl chloride group in the sulfonyl chloride resin Esterification is carried ou...
Embodiment 1
[0052] first step,
[0053] Mixture: at room temperature, add 1 g of sulfonyl chloride resin (Nankai Hecheng Co., Ltd., model: HC9001-1-1, sulfonyl chloride content: 1.78 mmol / g) and 25 mL of DCM into a 250 mL four-necked flask, Stir to swell to obtain a mixture.
[0054] Solution: Under ice bath, add 2.5 g of mPEG2000 and 50 mL of DCM to a 100 mL four-neck flask, and after the substrate is completely dissolved, add 30 mg of 4-dimethylaminopyridine (DMAP) and 4 mL of triethylamine. Continue stirring for 15 min.
[0055] The above mixture was placed in an ice bath, and the above prepared solution was slowly added dropwise to form a system to be reacted, and then the system to be reacted was slowly raised to room temperature for esterification reaction for 20 h to obtain a first product system. The first product system was filtered and washed with DCM and the washings recovered. The obtained resin is mPEG2000-sulfonyl chloride resin, and the resin weight increases to 1.37 g a...
Embodiment 2
[0062] first step,
[0063] Mixture: under ice bath, add 1 g of sulfonyl chloride resin (same as Example 1), 2 g of NaOH and 25 mL of THF to a 250 mL four-necked flask, stir and swell to obtain a mixture.
[0064] Solution: Under ice bath, add 2.5 g of mPEG2000 and 50 mL of THF to a 100 mL four-neck flask, and wait until the substrate is completely dissolved.
[0065] The above prepared solution was slowly added dropwise into the mixture to form the to-be-reacted system, and then the to-be-reacted system was slowly raised to room temperature to carry out the esterification reaction for 20 h to obtain the first product system. The first product system was filtered and washed with THF, and the washings were recovered. The obtained resin is mPEG2000-sulfonyl chloride resin, and the resin weight increases to 1.68 g after drying (resin weight gain is the grafting amount of mPEG2000). The product in this step has a purity of 100% and no further purification is required.
[0066] T...
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