The preparation method of polyethylene glycol dialdehyde derivative
A technology of polyethylene glycol and PEGylation, which is applied in the directions of non-active ingredients such as medical preparations, pharmaceutical formulations, aldehyde active ingredients, etc., can solve the problems of reducing the reaction conversion rate, decomposing the PEG chain and increasing the degree of distribution, etc. Achieving the effect of high purity and terminal activity
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preparation example 1
[0079]Preparation Example 1: Preparation of PEG-Ms
[0080]Make preparations for continuous flow of nitrogen into the reaction vessel, which is flame-dried to remove moisture. Add 100 g of PEG (Mn, about 3.4k) to the reaction vessel, and then add 300 ml of dichloromethane, and cool to 5°C after dissolving. Add 23.0 ml of triethylamine to the reaction solution and keep the temperature at 5°C, and then add 12.6 ml of methanesulfonyl chloride. The reaction solution was stirred at 5°C for 2.5 hours, 300 ml of distilled water was added, and then stirred for 10 minutes to separate the organic layer. 300 ml of dichloromethane was added to the water layer for further extraction, and then the organic layer was separated and combined. The organic layer was washed with 300 ml of distilled water, dried and filtered with anhydrous magnesium sulfate, and the filtrate was concentrated under reduced pressure. Add 100 ml of dichloromethane to the concentrate, add dropwise to 1500 ml of methyl tert-buty...
Embodiment 1
[0085]Example 1: Preparation of PEG-dialdehyde
[0086]Step (1): Preparation of PEG-diethyl acetal
[0087]Be prepared to keep nitrogen flowing into two 500 ml reaction vessels, which are flame-dried to remove water.
[0088]1.8 ml of 3,3-diethoxy-1-propanol and 40 ml of toluene were added to one of the reaction vessels. Then add 1.4 g of potassium tert-butoxide, wait until the temperature rises to 50°C, stir for 1 hour to activate the solution, and finally cool to room temperature.
[0089]10g of PEG-Ms obtained in Preparation Example 1 and 40 ml of toluene were added to another reaction vessel, the previously activated solution was added dropwise over 1 hour, and then stirred at room temperature for 2 hours. 50 ml of saturated ammonium chloride aqueous solution was added to the reaction solution, stirred for 5 minutes, 100 ml of dichloromethane was added, and the organic layer was extracted. 100 ml of dichloromethane was added to the water layer, the organic layer was further extracted, the ...
Embodiment 2
[0095]Example 2: Preparation of PEG-dialdehyde
[0096]Step (1): Preparation of PEG-diethyl acetal
[0097]Be prepared to keep nitrogen flowing into two 500 ml reaction vessels, which are flame-dried to remove moisture.
[0098]1.8 ml of 3,3-diethoxy-1-propanol and 40 ml of toluene were added to one of the reaction vessels. Then add 1.4g potassium tert-butoxide, wait for the temperature to rise to 50°C, stir for 1 hour to activate the solution, and cool to room temperature.
[0099]10 g of PEG-Ms obtained in Preparation Example 1 and 40 ml of toluene were added to another reaction vessel, and the previously activated solution was added dropwise over 1 hour, and then stirred at room temperature for 2 hours. 50 ml of saturated ammonium chloride aqueous solution was added to the reaction solution, and after stirring for 5 minutes, 100 ml of dichloromethane was added to extract the organic layer. 100 ml of dichloromethane was added to the water layer to further extract the organic layer, and the o...
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