Preparation method for aminophenol modified daiamid type tree shaped numerator

A polyamidoamine type, dendrimer technology, applied in the field of dendrimer preparation, can solve the problems of strong biological toxicity and long time, and achieve the effects of simple operation, stable performance and low price

Inactive Publication Date: 2009-01-14
SHANGHAI JIAO TONG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Its disadvantage is: the time required for the reaction is too long (7 days), the product carries

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Take 0.04mol of Fmoc and Pbf double-protected arginine, HOBt, HBTU, and 0.08mol of DIPEA and 0.01mol of hydroxyl-terminated G4 PAMAM dendrimers, dissolve them in 50ml of anhydrous DMF, and dissolve them at 37°C at 200r / min Stir the reaction for 12 hours, add anhydrous diethyl ether at 4°C until a large amount of precipitation precipitates, and obtain the precipitated crude intermediate product after suction filtration;

[0029] Take the crude intermediate product, dissolve it with a small amount of anhydrous DMF as a solvent, add the sample to Sephadex LH-20 column of Sephadex LH-20, and use anhydrous DMF as the mobile phase to elute. Water diethyl ether until a large amount of precipitation precipitates out, dissolve with 15ml of anhydrous DMF, repeat the diethyl ether precipitation method three times, and obtain a refined intermediate product after suction filtration;

[0030] Dissolve the refined intermediate product with 5ml of anhydrous DMF, add 45ml of trifluoroac...

Embodiment 2

[0032]Take 0.05mol of Fmoc and Pbf double-protected tryptophan, HOBt, HBTU, 0.09mol of DIPEA and 0.01mol of hydroxyl-terminated G4 PAMAM dendrimers, dissolve in 80ml of anhydrous DMSO, and stir at 25°C at 200r / min After reacting for 24 hours, add anhydrous diethyl ether at 4°C until a large amount of precipitation is precipitated, and the precipitated crude intermediate product is obtained after suction filtration;

[0033] Take the crude intermediate product, dissolve it with a small amount of anhydrous DMSO as a solvent, add the sample to the Sephadex LH-60 column of Sephadex LH-60, and use anhydrous DMSO as the mobile phase to elute, collect the eluate that flows out first, and add 4 °C without Water diethyl ether until a large amount of precipitation is separated out, and the refined intermediate product is obtained after suction filtration;

[0034] Dissolve the refined intermediate product in 6ml of anhydrous DMSO, add 50ml of trifluoroacetic acid, stir at 200r / min for 3...

Embodiment 3

[0036] Get 0.10mol of Fmoc and Pbf double-protected lysine, 0.04mol of HOBt, HBTU, and 0.07mol of DIPEA and 0.01mol of terminal hydroxyl G5 PAMAM dendrimers, mixed with 60ml of anhydrous DMF and anhydrous DMSO ( 1:1) was dissolved in the solvent, stirred and reacted at 200r / min at 25°C for 4h, added a mixed solution of anhydrous diethyl ether and anhydrous methyl ethyl ether (1:1) at 4°C until a large amount of precipitation was precipitated, and the precipitated product was obtained after suction filtration Crude intermediate products;

[0037] Get the crude product intermediate product, dissolve with the mixed solution (1:1) of a small amount of anhydrous DMF and anhydrous DMSO as solvent, add sample on Sephadex LH-20 column of Sephadex, with anhydrous DMF and anhydrous DMSO The mixed solution (1:1) was used as the mobile phase for elution, and the eluent that flowed out first was collected, and a mixed solution (1:1) of anhydrous diethyl ether and anhydrous methyl ethyl eth...

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PUM

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Abstract

The invention discloses a preparation method for dressing polyamidoamine dendrimer by amino acid. The reaction is performed in organic solvent, hydroxyl benztriazole HOBt, 2-(1H-benzotriazole)-N, N N`, N`-tetramethyluroniumhexafluorophosphate HBTU, N and N-diisopropylethylamine DIPEA are taken as catalyzer, to ensure that 2, 2, 4, 6 and 7-pentamethyldihydrobenzofuran-5-sulfonyl Pbf and 9-fluorenylmethyloxycarbonyl Fmoc dual-protection amino acid and terminal hydroxyl group PAMAM dendrimer can generate the condensation reaction. The refinement is performed through adopting dextran gel chromatography, to ensure that trifuoroacetic acid and piperidine can respectively divest of the Pbf protecting group and the Fmoc protecting group of the amino acid and the depurant amino acid can be obtained to dress the PAMAM dendrimer of the terminal hydroxyl group. The operation of the preparation method is simple, the condition is moderate, the price is low, the purer end product can be obtained, the preparation process can not damage the activation of the guanidino in the amino acid, and the preparation method is suitable for a great quantity of preparation and industrialized production.

Description

technical field [0001] The invention relates to a preparation method of a dendrimer in the technical field of chemical engineering, in particular to a preparation method of an amino acid modified polyamidoamine type (PAMAM) dendrimer. Background technique [0002] Dendrimer is a new type of synthetic polymer with three-dimensional spherical shape and high order, which is currently under vigorous development. In terms of structure, it has the characteristics of high geometric symmetry, precise molecular structure, a large number of surface terminal functional groups that can be modified, controllable intramolecular cavity and molecular chain length, simple preparation method, and low cost. Its appearance is a shock to the classical organic polymer world. It is the intersection of chemistry, life science and material science, and has become a major research hotspot in the current academic circle. Due to the highly branched structure and unique monodispersity of dendrimers, a ...

Claims

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Application Information

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IPC IPC(8): C08G69/48C08G73/02
Inventor 宋华崔大祥高峰贺蓉
Owner SHANGHAI JIAO TONG UNIV
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