Preparation method for aminophenol modified daiamid type tree shaped numerator
A technology of hydroxyl-terminated polyamidoamine type and polyamidoamine type, which is applied in the field of preparation of dendrimers, can solve the problems of strong biological toxicity and long time, and achieve the effect of simple operation, stable performance and precise structure
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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 G4PAMAM dendrimers, dissolve in 50ml of anhydrous DMF, and stir at 200r / min at 37°C After reacting for 12 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;
[0029] Take the crude intermediate product, dissolve it in a small amount of anhydrous DMF, add the sample to Sephadex LH-20 column of Sephadex LH-20, use anhydrous DMF as the mobile phase to elute, collect the eluate that flows out first, add 4 °C without 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...
Embodiment 2
[0032]Take 0.05 mol of Fmoc and Pbf double-protected tryptophan, HOBt, HBTU, and 0.09 mol of DIPEA and 0.01 mol of hydroxyl-terminated G4PAMAM dendrimers, dissolve in 80ml of anhydrous DMSO, and stir at 25°C at 200r / min for reaction After 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...
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 G5PAMAM dendrimers, with the mixed solution of 60ml anhydrous DMF and anhydrous DMSO (1 : 1) for solvent dissolution, stirring and reacting at 200r / min at 25°C for 4h, adding a mixed solution (1:1) of anhydrous diethyl ether and anhydrous methyl ethyl ether at 4°C until a large amount of precipitation is precipitated, and the precipitated crude product is obtained after suction filtration mid product;
[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, apply on the Sephadex LH-20 post of Sephadex gel, add anhydrous DMF and anhydrous DMSO The mixed solution (1:1) is the mobile phase elution, collect the eluent that flows out first, add the mixed solution (1:1) of anhydrous diethyl ether and anhydrous methyl ethyl ether at 4°C until a large...
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