Electric Literature of 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.
Compound B (5356 kg) was suspended in a mixture of acetic anhydride and acetic acid (7760 L, 1.45 L/kg Compound B, 87 v/v % acetic anhydride and 13 v/v % acetic acid) at ambient temperature. This mixture was prepared by mixing acetic anhydride (6086 kg) and regenerated acetic anhydride (2295 kg), the latter containing 48 v/v % acetic anhydride and 52 v/v % acetic acid obtained from a previous batch. The mixture was heated to 55C. Then, p-toluene sulfonic acid (25 kg) was added and the reaction mixture was further heated to 124C over about 90 minutes. All solids were dissolved in the reaction, and 100 % of Compound B was acetylated. The remaining acetic anhydride/acetic acid (5580 L) was distilled off under reduced pressure resulting in a very viscous reaction mixture. Thirty-nine percent of the distillate could be re-used as reagent in a later batch without a discrete purification step.
The basis of chemical reaction formula synthesis, the synthesis route is composed of some specific reactions and combined according to certain logical thinking. We look forward to the emergence of more reaction modes in the future.