Method of preparing branched polyethylene glycol
A polyethylene glycol and branched technology, which is applied in the fields of biomedicine and protein chemistry, can solve the problems of biodegradation, difficult control of reaction conditions, high price of branched polyethylene glycol, etc., and achieves high yield and high price. cheap effect
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Embodiment 1
[0043] Embodiment 1, prepare a kind of branched polyethylene glycol with the method of the present invention, its step is:
[0044] 1. Preparation of lysine ethyl ester hydrochloride
[0045] Dissolve L-lysine in absolute ethanol, feed dry hydrogen chloride gas to saturation under stirring conditions, heat to reflux to dissolve L-lysine, and leave the solution overnight; then distill under reduced pressure to remove excess ethanol and hydrogen chloride ; Finally, carry out crystallization of ethyl lysine hydrochloride with anhydrous ether; then filter, wash, and dry to obtain light yellow crystals of ethyl lysine hydrochloride;
[0046] 2, the preparation molecular weight is the carboxymethylated monomethoxy polyethylene glycol of 5000
[0047] Dissolve mPEG5000 in dry dichloromethane, add activated manganese dioxide, mix evenly, and stir overnight at room temperature; filter to remove the catalyst, and evaporate the solvent under reduced pressure to obtain an intermediate ox...
Embodiment 2
[0054] Embodiment 2, prepare a kind of branched polyethylene glycol with the method of the present invention, its step is:
[0055] 1. Preparation of lysine ethyl ester hydrochloride
[0056] Dissolve L-lysine in absolute ethanol (1:8 molar ratio), feed dry hydrogen chloride gas to saturation under stirring conditions, heat to reflux to dissolve L-lysine, and leave the solution overnight; then reduce Pressure distillation removes excess ethanol and hydrogen chloride; Finally, carry out the crystallization of ethyl lysine hydrochloride with anhydrous ether; then filter, wash, and dry to obtain light yellow crystals of ethyl lysine hydrochloride;
[0057] 2. Preparation of molecular weight is 2000 carboxymethylated monomethoxypolyethylene glycol
[0058] Dissolve 25 grams of mPEG2000 in dry dichloromethane, add 20 grams of activated manganese dioxide, mix uniformly, and stir overnight at room temperature; filter to remove the catalyst, and evaporate the solvent under reduced pr...
Embodiment 3
[0065] Embodiment 3, prepare a kind of branched polyethylene glycol with the method of the present invention, its step is:
[0066] 1. Preparation of lysine ethyl ester hydrochloride
[0067] Dissolve L-lysine in absolute ethanol, feed dry hydrogen chloride gas to saturation under stirring conditions, heat to reflux to dissolve L-lysine, and leave the solution overnight; then distill under reduced pressure to remove excess ethanol and hydrogen chloride ; Finally, carry out crystallization of ethyl lysine hydrochloride with anhydrous ether; then filter, wash, and dry to obtain light yellow crystals of ethyl lysine hydrochloride;
[0068] 2. Preparation of molecular weight is 750 carboxymethylated monomethoxypolyethylene glycol
[0069] Dissolve mPEG750 in dry dichloromethane, add activated manganese dioxide, mix evenly, and stir overnight at room temperature; filter to remove the catalyst, and evaporate the solvent under reduced pressure to obtain an intermediate oxidation pro...
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