Method of preparing carboxylic acid functionalized polymers
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example 1
mPEG(30,000)-carboxylic acid
[0161] A solution of mPEG-30,000 (50 g, 0.00167 moles) (NOF Corporation) in toluene (600 ml) was azeotropically dried by distilling off 300 ml toluene. t-Butanol (70 ml), potassium tert-butoxide (95%, 1.75 g, 0.0148 moles, 8.9 fold excess) and tert-butyl bromoacetate (3.3 g, 0.0169 moles, 10.1 fold excess) were added, and the mixture was stirred overnight at 45° C. under argon atmosphere. The solvent was distilled off under reduced pressure, and the residue was dissolved in distilled water (1000 ml).
[0162] The pH of the aqueous solution was adjusted to 12 with 1 M sodium hydroxide, and the solution was stirred for 18 h, keeping the pH at 12 by periodic addition of 1M sodium hydroxide.
[0163] The pH was adjusted to 3 with 5% phosphoric acid, and the product was extracted with dichloromethane. The extract was dried with anhydrous magnesium sulfate and added to ethyl ether. The precipitated product was filtered off and dried under reduced pressure, giving ...
example 2
PEG(10,000)-dicarboxylic acid
[0166] PEG-10,000 (35.25 g, 0.00705 eq) (NOF Corporation) (terminated at both ends with hydroxyl) was dissolved in toluene (600 ml) and azeotropically dried by distilling off toluene. The residue was redissolved into anhydrous toluene (500 ml). tert-Butanol (40 ml), potassium tert-butoxide (4 g, 0.0356 moles, 5.1 fold excess) and anhydrous toluene (40 ml) were combined and added to the above reaction mixture, followed by stirring for about 3.5 hours. t-Butyl bromoacetate (7 ml, 0.0474 moles, 6.7 fold excess) was added, and the mixture was stirred overnight at 40° C. under argon atmosphere. The solvent was distilled off under reduced pressure, and the residue was dissolved in distilled water (1000 ml).
[0167] The pH of the aqueous solution was adjusted to 12.1 with 1M sodium hydroxide, and the solution was stirred overnight, keeping the pH at 12.1 by periodic addition of 1M sodium hydroxide.
[0168] The pH was adjusted to 1.0 with 1M hydrochloric acid, an...
example 3
PEG(5,000)-dicarboxylic acid
[0171] A solution of PEG-5,000 (35 g, 0.01400 equivalents) (NOF Corporation) in acetonitrile (800 ml) was azeotropically dried by distilling off acetonitrile, and the residue was redissolved into anhydrous toluene (300 ml). t-Butanol (50 ml), potassium tert-butoxide (4.7 g, 0.0419 moles, 2.99 fold excess), and anhydrous toluene (50 ml) were combined and added to the above reaction mixture, followed by about 3.5 hours of stirring. t-Butyl bromoacetate (7.2 ml, 0.0488 moles, 3.48 fold excess) was added, and the mixture was stirred 20 hrs at room temperature under an argon atmosphere. The solvent was distilled off under reduced pressure, and the residue was dissolved in distilled water (1000 ml).
[0172] The pH of the aqueous solution was adjusted to 12.0 with 1M sodium hydroxide, and the solution was stirred overnight, keeping the pH at 12.0 by periodic addition of 1M sodium hydroxide.
[0173] The pH was adjusted to 2.0 with 1M hydrochloric acid and the prod...
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