Electric Literature of 76801-93-9, In the next few decades, the world population will flourish. As the population grows rapidly and people all over the world use more and more resources, all industries must consider their environmental impact. 76801-93-9, name is 5-Amino-N1,N3-bis(2,3-dihydroxypropyl)-2,4,6-triiodoisophthalamide belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.
Example 1Ten experiments were made, each of which used two parallel crystallisers (reactors A and B) where one had mother liquor distilled off and one had not. The solutions of crude Compound A were in all cases made the following way.Compound B was acetylated by a mixture of acetic anhydride and acetic acid (concentration about 91 v/v %, 2.0 L/kg Compound B) at 50-125 C. in the presence of catalytic amounts of p-toluene sulphonic acid. Excess acetic anhydride and acetic acid were distilled off under reduced pressure, and the resulting viscous solution diluted with methanol and water and hydrolysed by addition of aqueous sodium hydroxide at 50-60 C. to a stable pH of about 12. Hydrochloric acid (17.5 w/w %) was added to a pH of about 10.5-11.5 at 60 C. Then, seeds of crystalline Compound A (0.004 kg/kg Compound B) were added, and pH was further adjusted to 6.5-7.5 by hydrochloric acid (17.5 w/w %). At this stage the solvent composition was approximately 25% methanol and 75% water, with a total mother liquor volume of about 3.8 L/kg Compound A.In reactor A of each experiment a certain fraction of the mother liquor volume was removed by distillation, either at atmospheric or reduced pressure (95-100 C. at atmospheric pressure, 55-60 C. under reduced pressure). In reactor B nothing was distilled off. The content of both reactors were then allowed to cool gradually to 15 C. over 10-12 hours before filtration, wash with methanol and drying under reduced pressure and elevated temperature. The purity of the crystals was measured by HPLC. The following results were obtained: Water Reduction Water Reduction Isolated content in of mother content in of mother yield mother Compound liquor mother Compound liquor increase, liquor, B purity, volume, liquor, B purity, volume, reactor B vs. reactor A reactor A reactor A reactor B reactor B reactor B reactor A 1 81% 99.6% 11% 76% 99.6% None 1.3% 2 84% 99.6% 11% 76% 99.6% None 1.4% 3 85% 99.5% 14% 78% 99.5% None 1.7% 4 84% 99.5% 17% 73% 99.6% None 1.9% 5 83% 99.5% 14% 75% 99.5% None 1.6% 6 88% 99.5% 27% 77% 99.4% None 2.9% 7 91% 99.5% 24% 80% 99.5% None 2.5% 8 89% 99.5% 36% 76% 99.5% None 2.9% 9 85% 99.4% 28% 74% 99.5% None 2.4% 10 89% 99.4% 32% 75% 99.5% None 3.1%
In the field of chemistry, the synthetic routes of compounds are constantly being developed and updated. I will also mention this compound in other articles, 5-Amino-N1,N3-bis(2,3-dihydroxypropyl)-2,4,6-triiodoisophthalamide, other downstream synthetic routes, hurry up and to see.
Reference:
Patent; GE HealthCare AS; US7754920; (2010); B1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com