Triple-bond pendant-group aliphatic poly (ester-carbonic ester) and preparation method thereof
An aliphatic and carbonate technology, which is applied in the preparation method of peptides, chemical instruments and methods, and pharmaceutical formulations, can solve the problems of complex synthesis process and high cost, and achieve the effect of high reactivity
- Summary
- Abstract
- Description
- Claims
- Application Information
AI Technical Summary
Problems solved by technology
Method used
Image
Examples
Embodiment 1
[0026] Example 1: Synthesis of 2-methyl-2-propargyloxycarbonyl-1,3-propanediol
[0027] 9.00 g of 2,2-dimethylolpropionic acid and 4.30 g of potassium hydroxide were dissolved in 50 ml of N,N-dimethylformamide. Stir vigorously for 1 h at 100°C to form potassium salt of 2,2-dimethylolpropionate. Then propargyl bromide was added to the above solution, and stirred vigorously at 100°C for 15h. The solvent was distilled off, the residue was dissolved in 200 ml of ether, washed three times with 50 ml of distilled water, and finally recrystallized with toluene to obtain 8 g of 2-methyl-2-propargyloxycarbonyl-1,3-propanediol with a yield of 70%. Its structure was confirmed by proton NMR spectroscopy.
Embodiment 2
[0028] Embodiment 2: the synthesis of 2-methyl-2-propargyloxycarbonyl trimethylene carbonate (monomer A)
[0029] Dissolve 10 g of 2-methyl-2-propargyloxycarbonyl-1,3-propanediol and 28.5 g of ethyl chloroformate in 600 ml of tetrahydrofuran, and cool in an ice-water bath. Then slowly add 28g of triethylamine into the above solution, and keep the system at about 0°C during the addition. Then react at room temperature for 10h. The precipitate was filtered off, the filtrate was concentrated under reduced pressure, and the residue was recrystallized from tetrahydrofuran and diethyl ether to obtain 9.4 g of white crystals with a yield of 82%. Its structure was confirmed by proton NMR spectroscopy.
Embodiment 3
[0030] Embodiment 3: the synthesis of the copolymer of monomer A and lactic acid
[0031] Under anhydrous and oxygen-free conditions, add 0.2 mole of monomer A and 0.8 mole of lactide monomer into the polymerization reaction bottle, and then add ethyl zinc of 1 / 200 of the total mass of the monomer as an initiator, at 60 The reaction was stirred at ℃ for 2 hours, the product was dissolved in chloroform, precipitated in methanol, filtered, washed, dried in vacuum at 35 ℃ for 24 hours, and the yield was calculated by weighing to obtain a copolymer of monomer A and lactic acid. The weight yield is 89%, and the weight average molecular weight is 1.56×10 4 , molecular weight distribution index 1.15.
PUM
| Property | Measurement | Unit |
|---|---|---|
| molecular weight distribution | aaaaa | aaaaa |
| molecular weight distribution | aaaaa | aaaaa |
| molecular weight distribution | aaaaa | aaaaa |
Abstract
Description
Claims
Application Information
Login to View More 