1021298-68-9, 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. 2-Fluoro-5-((4-oxo-3,4-dihydrophthalazin-1-yl)methyl)benzonitrile, cas is 1021298-68-9,the phthalazine compound, it is a common compound, a new synthetic route is introduced below.
Add Compound III 25.82 g to the reaction flask.Purified water 100ml,Stir at room temperature,Then add 22.4M sodium hydroxide 92.4ml,The mixture temperature was heated to 100 C,Stir 12h, cool to room temperature, filter, wash,The combined filtrate was acidified with 46.2 ml of 2M diluted hydrochloric acid for 30 min,Then, 500 ml of methanol, 18.70 g of triethylamine, and 14.25 g of 1-cyclopropanecarbonylpiperazine are added successively.At a reaction temperature of 20-25C, the reaction is stirred for 10 hours. After the reaction is completed, it is cooled to 0C and filtered.38.66 g of solids were obtained with a yield of 96.2% and a purity of 99.89%. The refining of olaparib (I)30g of crude oleapani was placed in a dissolving tank81.82 ml of isopropanol and 818.2 ml of acetone were added and the temperature was controlled at 45-50C.Stir and dissolve. After the crude product is completely dissolved, add charcoal to decolorize it for 30 minutes.The decolorization reaction was followed by hot filtration and the filtrate was stirred at room temperature for crystallization.Then cool down to 0 ~ 10 C for 4 hours, filter, and wash with acetone,Filtration, drying, that is, olaparib 28.35g,The yield was 94.5%, the purity was 99.99%, the mononuclear 0.05%, and the total heterologous 0.11%.
Other significant industrial processes that involve the use of heterogeneous catalysts include the preparation of sulfuric acid, the preparation of ammonia, the oxidation of ammonia to nitric acid, and the synthesis of methanol.1021298-68-9, if you are interested, you can browse my other articles.
Reference£º
Patent; Shandong Yuxin Pharmaceutical Co., Ltd.; Liu Zhenteng; Chen Yu; Sun Heng; Wang Chunyan; (6 pag.)CN108101852; (2018); A;,
Phthalazine – Wikipedia
Phthalazine | C8H6N2 – PubChem