5 Amino 2,4,6 triiodoisophthalic acid was synthesized from isophthalic acid by a three step procedure,nitration,reduction and iodination. (1)Nitration:at n (sulfuric acid)∶ n (sodium nitrate)∶ n (isophthalic acid)=7 9∶2 2∶1 0 after reacting at 60 ℃ for 3 h,the yield of nitro compound was 86.7%.
By using GPC/Viscometry, the calculation of intrinsic viscosity can be simplified, and the absolute molecular weight and its distribution of polyaspartic acid are quickly determined,too. The largest error is in the range of 1.02%~4.2%,and the value of K is 1.09×10~ -3 dL/g and α is 0.40 in the 0.1KG-*9mol/L sodium nitrate solution at 35℃.
The result shows that it is better to control the reaction temperature of trifluoroaniline sulfate preparation and sodium nitrate dropping addition are 55 ℃ and 15 ℃ during diazotization, respectively;
(1)Nitration:At n (sulfuric acid)∶ n (sodium nitrate)∶ n (isophthalic acid)=7.9∶2 2∶1 0(at 60℃)for 3h,the yield of nitrate is 86 1%,(2)Reduction:At n (iron)∶ n (nitrate)=3.0∶1 0 after being refluxing for 3 h,the yield of aminate is 77 2%;
The sol coagulation thresholds are determined in the presence of sodium nitrate and sulfate, as well as of mixed magnesium salt at various pH values of the dispersion medium.
New nanocomposites based on zeolites (NaA-NaNO2, NaA-NaNO3) and opals (o-NaNO2, o-NaNO3) that contain sodium nitrite or sodium nitrate nanoparticles in cages of regular porous matrices are prepared.
Phenol was directly nitrated in two phases consisted of diethyl ether and aqueous sodium nitrate-sulfuric acid solution. The yield of nitrated product is more than 80%. No obvious oxidation product was formed in reaction. The recovery of diethyl ether is more than 75%.
In the two-phase nitration of phenol in the persence of β-CD,the regioselectivity of the reaction could be improved markedly,factors such as the polarity of the organic solvents,the amount of sodium nitrate used and reaction temperature have been investigated.Some experimental results have been discussed.
Chloro-2-methylbenzimidazole 1 was Synthesized. Acetanilide reacted with chlorine in acetic acid/water to offer 4-chloro-acetanilide 5 in yield of 67.3%. 5 was nitrated with sodium nitrate/sulfuric acid/sodium nitrite at 0~15℃ to give 5-chloro-2-nitroacenilide 6 in yield of 70. 8%. Reduction of 6 with Hcl-HOAc/Fe followed by cyclization furnished 1 in yield of 78.4%. Effects of different reaction conditions on yield of products mentioned above were studied and the results of the expe...