132812-72-7Relevant articles and documents
An investigation into formation of impurities during synthesis of blonanserin
Sudarshan Rao,Nageswara Rao,Uma Sankara Sastry,Muralikrishna,Jayashree
, p. 5928 - 5930 (2014)
During the process development of Blonanserin (1 ), we have observed formations of unknown impurities are in the final product at enhanced levels which was identified as Des ethyl impurity, di-N-ethylpiperazine impurity, Chloro impurity and des-fluoro impurity. The present work involves detailed optimization studies directed toward the development of an efficient process for the commercial production of Blonanserin substantially free from the chloro impurity and other impurities.
High-efficiency preparation method of blonanserin intermediate
-
Paragraph 6-9, (2019/12/25)
The invention discloses a high-efficiency preparation method of a blonanserin intermediate (BN-03). The method comprises the following two steps: (1) hydrolyzing p-fluorobenzoylacetonitrile by using 30% hydrogen peroxide in the presence of a composite catalyst composed of a heteropoly acid (a heteropoly acid salt) and a phase transfer catalyst under basic conditions in an organic solvent so as togenerate 3-(4-fluorophenyl)-3-oxo-propionamide; and (2) performing a reaction on 3-(4-fluorophenyl)-3-oxo-propionamide and cyclooctanone under the catalysis of an acid in at least one organic solventso as to obtain 4-(4-fluorophenyl)-5,6,7,8,9,10-hexahydrocycloocta[b]pyridine-2(1H)-one. The total yield of the product is increased from 63.5% to about 85%.
Synthetic method for Blonanserin
-
, (2017/01/12)
The invention discloses a synthetic method for Blonanserin. The synthetic method comprises the following steps: 1) methyl fluorobenzoate is taken as a raw material and subjected to condensation with acetonitrile, and a compound 3 is obtained; 2) polyphosphoric acid is heated, then the compound 3 and a cyclooctanone and an ionic liquid are added, and a compound 4 is obtained through a one-step reaction; 3) the compound 4 is subjected to chlorination through a phenylphosphonic dichloride compound, and a compound 5 is obtained; 4) the compound 5 is mixed with potassium iodide and 1-ethylpiperazine, the ionic liquid is added, heating and nucleophilic substitution are performed, and Blonanserin is obtained, wherein the ionic liquid in the step 2) and the step 3) is 1-ethyl-3-methylimidazolium tetrafluoroborate, the adding quantity of the ionic liquid in the step 2) is 30% of the mass of the compound 3, and the adding quantity of the ionic liquid in the step 3) is 30% of the mass of the compound 5. Compared with the conventional synthetic method for Blonanserin, the synthetic method has the advantages that the reaction time is shortened greatly, the yield is increased, the production cost is reduced, and the method is applicable to industrial production.