134450-56-9, name is 4,5-Difluorophthalonitrile, belongs to nitriles-buliding-blocks compound, is considered to be a conventional heterocyclic compound, which is widely used in drug synthesis. The chemical synthesis route is as follows. Recommanded Product: 134450-56-9
1.52 g (9.14 mmol) 9H-carbazole and 1.91 g (13.7 mol)of potassium carbonate were placed in a 50-mE recovery flask, and the interior of the flask was substituted with nitrogen. 15 mE of dimethylsulfoxide was added to themixture, which was stirred under a nitrogen stream at room temperature for 1 hout 0.500 g (3.05 mmol) of 4,5-difluo- rophthalonitrile was added to the mixture. The mixture was stirred under a nitrogen stream at room temperature for 3 hours and then at 500 C. for 20 hours. Thereafier, the mixturewas added to water, followed by stirring. The mixture was extracted with toluene. After the extraction, the extracted solution was rinsed with a saturated sodium chlorine aqueous solution. After rinsing, an organic layer and an aqueous layer were separated, and the organic layer was dried byadding magnesium sulfate thereto. After drying, the mixture was suction-filtered to provide a filtrate. The resulting filtrate was concentrated to provide a solid matter, which was purified by silica gel column chromatography. In the purification, a mixed solvent of toluene and hexane (1/4) was firstly used as a developing solvent, then a mixed solvent of toluene and hexane (7/3) was used, and then toluene was used as a developing solvent (the developing ratio was gradually changed). The resulting fraction was concentratedto provide a solid matter, which was then rinsed by reslurrywith a mixed solvent of acetone and methanol, therebyproviding a pale yellow powdered solid matter in a yieldamount of 1.20 g and a yield of 85.8%.
The synthetic route of 134450-56-9 has been constantly updated, and we look forward to future research findings.
Reference:
Patent; KYULUX, INC.; Adachi, Chihaya; Uoyama, Hiroki; Nomura, Hiroko; Goushi, Kenichi; Yasuda, Takuma; Kondo, Ryosuke; Shizu, Katsuyuki; Nakanotani, Hajime; Nishide, Jyunichi; (83 pag.)US9502668; (2016); B2;,
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