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