Tag: M.W=700-800

As we all know, there are many different methods for the synthesis of a compound, and people can choose the synthesis method that suits their own laboratory according to the actual situation. 76801-93-9 name is 5-Amino-N1,N3-bis(2,3-dihydroxypropyl)-2,4,6-triiodoisophthalamide, This compound is widely used in many fields, so it is necessary to find a new synthetic route. The downstream synthesis method of this compound is introduced below. 76801-93-9

In Example 2, the solution was cooled in a reactor jacket to 70 C immediately after reaching the maximum temperature of approximately 120-125 C. The cooling rate was about 1 C/minute, and the solution was held at 70 C overnight to form over-acetylated Compound A before moving on to the next deacetylation process step to form Compound A. Deacetylation: After acetylation, the reaction solution containing over-acetylated Compound A was concentrated under reduced pressure, before methanol and water was added prior to the deacetylation step. Sodium hydroxide was then added to methanol- water reaction mixture to carry out the deacetylation. The resulting reaction mixture was then further diluted with water before crystallization. Crystallization: To achieve crystallization, hydrochloric acid was first added until the reaction mixture until it was slightly turbid, and then the reaction mixture was seeded with Compound A. The resulting slurry was stirred for 45 minutes before additional hydrochloric acid was added until about pH 7. The slurry was then cooled to 15 C over night. Next day the slurry was filtered, and the filter cake was washed with methanol and then dried in a vacuum oven.

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 5-Amino-N1,N3-bis(2,3-dihydroxypropyl)-2,4,6-triiodoisophthalamide, and friends who are interested can also refer to it.

Reference:
Patent; GE HEALTHCARE AS; SAANUM, Inger, Dagny; HAALAND, Torfinn; KALLEBERG, Rita; WO2015/82719; (2015); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

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. 76801-93-9

The white powdery product S4 (10 g, 14.2 mmol) obtained in Example 3.Dissolved in 20mL DMAc and acetonitrile mixture (1:1 volume ratio),Cool down to 10 C, control temperature below 30 C,3-chloropropanediol-(1,2) or 2-chloroethanol-1 (10.2 g, 92.3 mmol) was added dropwiseOr 9.55g, 92.3mmol), after the addition is completed, the temperature is raised to 50 C,After stirring for 3 h, it was cooled to 15 C, 20 mL of 10 mol/L NaOH aqueous solution was added dropwise, and the reaction was further stirred at 25 C for 1 h. After the reaction was completed, the pH was adjusted to 4 with dilute hydrochloric acid.Allow to stand at 0 C overnight, filter, filter cake washed with water several times,Drying (drying to constant weight at 85 C),Recrystallization (recrystallization in DMAc mixed with acetonitrile),A white gray or dark gray powder compound is obtained.

The synthetic route of 76801-93-9 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; China Calculate University; Wu Zhiping; Bai Xueyan; Wu Yuqi; (13 pag.)CN108727376; (2018); A;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

A common heterocyclic compound, 76801-93-9, name is 5-Amino-N1,N3-bis(2,3-dihydroxypropyl)-2,4,6-triiodoisophthalamide, molecular formula is C14H18I3N3O6, its 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. 76801-93-9.

5-amino-N,N’-bis(2,3-dihydroxypropyl)-2,4,6-triiodoisophthalamide (500 g) was taken in N-methylpyrrolidone (500 ml). Chloroacetyl chloride (500 ml) was then added over three hours maintaining the temperature below 35 0C. After addition, the reaction mixture was stirred for three hours at 50 0C. Water (1.3 L) was added to the reaction mass and the precipitated product was filtered, washed and dried. Yield: 97%Purity: 96% (by HPLC)

The synthetic route of 5-Amino-N1,N3-bis(2,3-dihydroxypropyl)-2,4,6-triiodoisophthalamide has been constantly updated, and we look forward to future research findings.

Reference:
Patent; WOCKHARDT RESEARCH CENTRE; KULKARNI, Dilip, Ganesh; SINHA, Rohit, Kumar; SHINDE, Prakash, Sakharam; SIDDIQUI, Mohammed, Jaweed, Mukarram; ZAKIR, Gafoor, Shaikh; MOHAMMED, Ismail, Shafi; ANIS, Mushtaqe, Ali, Saiyad; KHAN, Nasim; WO2008/104853; (2008); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Adding some certain compound to certain chemical reactions, such as: 73334-07-3, name is N1,N3-Bis(2,3-dihydroxypropyl)-2,4,6-triiodo-5-(2-methoxyacetamido)-N1-methylisophthalamide, can increase the reaction rate and produce products with better performance than those obtained under traditional synthetic methods. Here is a downstream synthesis route of the compound 73334-07-3. 73334-07-3

12,000 g of iopromide, pure mother liquor (solid content about 6.2%), is concentrated by evaporation in a vacuum to form viscous oil of 892 g. 877 g of this residue is mixed in a suitable reaction vessel at a bath temperature of 65 C. with 439 ml of 1-propanol while being stirred. After inoculation with 0.73 g of iopromide, it is fully stirred for another 48 hours at a bath temperature of 65 C. The crystal suspension is then cooled to 20 C., stirred for I hour at this temperature and suctioned off via a suction filter. After washing with 4 portions of 110 ml of ethanol, the secondary crystallizate is dried at 40 C. in a vacuum-drying oven. Yield: 363.8 g (about 52% of the experiment)

Chemical properties determine the actual use. Each compound has specific chemical properties and uses. We look forward to more synthetic routes in the future to expand reaction routes of N1,N3-Bis(2,3-dihydroxypropyl)-2,4,6-triiodo-5-(2-methoxyacetamido)-N1-methylisophthalamide.

Reference:
Patent; Kagerer, Hartmut; Dembeck, Meike; Seba, Harmut; Ortmann, Ingo; US2007/265470; (2007); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

76801-93-9, A common heterocyclic compound, 76801-93-9, name is 5-Amino-N1,N3-bis(2,3-dihydroxypropyl)-2,4,6-triiodoisophthalamide, molecular formula is C14H18I3N3O6, its 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.

EXAMPLES EXAMPLE 1; 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 50-125C. 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 HPLC Compound B: 0.0-0.3 % by area in HPLC Concentration: 31 w/v % Compound A in an approximately 2.5:1 methanol/water mixture Conductivity: 5.1-5.7 mS/cm Compound B was produced from the reaction mixture in a system according to Figure 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 55C (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 60C in the two first crystallisers and 20C 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 120-130C gas temperature. The maximum temperature exposed to the product was 80C. The resulting moisture content was 0.4 w/w %. The purity of dry Compound A in HPLC was 99.5 % by area.

The synthetic route of 76801-93-9 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; GE Healthcare AS; EP2281811; (2011); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com