Related Products of 76801-93-9,Some common heterocyclic compound, 76801-93-9, name is 5-Amino-N1,N3-bis(2,3-dihydroxypropyl)-2,4,6-triiodoisophthalamide, molecular formula is C14H18I3N3O6, traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route.
Compound B was acetylated in a mixture of acetic anhydride and acetic acid in the presence of catalytic amounts of p-toluene sulphonic acid at 50-125 C. Excess acetic anhydride and acetic acid was distilled off under reduced pressure, and the reaction mixture was diluted with methanol and water. The resulting reaction mixture had the following composition:Overacetylated Compound A (a mixture of compounds with varying number of acetyl groups attached): 97.7-98.3% by area in HPLCCompound B: 0.0-0.3% by area in HPLCConcentration: 31 w/v % Compound A in an approximately 2.5:1 methanol/water mixtureConductivity: 5.1-5.7 mS/cmCompound B was produced from the reaction mixture in a system according to FIG. 1. The reaction mixture from the acetylation reaction (prepared batch wise) was fed into the static mixer in a flow ratio of 1.04 mL reaction mixture:1.0 mL 20 w/w % NaOH at about 55 C. (outlet temperature). The absolute feeding rate of the reaction mixture was 2.6 kg/hour. The pH was kept at about 12.2 at steady state. HPLC of the output stream showed Compound A in 98.2% purity with 0.23% Compound B present at steady state.The continuous crystallisation was performed as described above. The pH in the first and second crystalliser varied between 11.1 and 11.5 over time, while the pH in the third and fourth crystalliser varied between 6.2 and 7.2. The temperature was 60 C. in the two first crystallisers and 20 C. in the third and fourth. Residence times were held at 2, 2, 2 and 8 hours, respectively. 20% of the mother liquor volume was stripped off in the third crystalliser at a pressure of 240-250 mbar. The water content in the methanolic distillate from the stripping was 34-35 w/w %. The resulting slurry from the fourth crystalliser was transferred to a holding tank before filtration.The slurry was filtered in a continuous rotation filter at 1.6-3.2 barA. The filtration rate varied between about 500 and 900 L/m2/hour (about 500-650 L/m2/hour at steady state). The filter cake was washed with methanol (about 1.9 kg/kg Compound A) in the same filter. The resulting salt content in the filter cake was 0.2-0.3 w/w % NaCl.The moist filter cake was dried in a continuous fluid bed (spin flash) dryer at 120-130 C. gas temperature. The maximum temperature exposed to the product was 80 C. The resulting moisture content was 0.4 w/w %.The purity of dry Compound A in HPLC was 99.5% by area.
These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 5-Amino-N1,N3-bis(2,3-dihydroxypropyl)-2,4,6-triiodoisophthalamide, its application will become more common.