108-70-3, name is 1,3,5-Trichlorobenzene, belongs to chlorides-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. Application In Synthesis of 1,3,5-Trichlorobenzene
Synthesis Example 5 Synthesis of 1,3,5-Trichloro-2,4,6-tris(phenylethynyl)benzene (corresponding to Scheme 3-(8)) [Show Image] Under a nitrogen atmosphere, in a 100 mL three-neck flask, 1,3,5-trichloro-2,4,6-triiodobenzene (5.0 g, 8.94 mmol) obtained in Synthesis Example 1, diisopropylamine (4.5 mL) and THF (40 mL) were placed and degassed by Ar bubbling for 30 minutes. Pd(PPh3)4 (200 mg, 0.17 mmol), CuI (310 mg, 1.6 mmol) and ethynyl benzene (3.92 mL, 35.8 mmol) were added and refluxed for 20 hours. After the reaction was terminated with a 1N hydrochloric acid solution (20 mL), the reaction mixture was extracted with methylene chloride (50 mL x 3), washed with an aqueous sodium hydrogen carbonate solution (150 mL x 1) and saturated saline solution (150 mL x 2) and dried over anhydrous magnesium sulfate. After the solvent was distilled away under reduced pressure, a by-product(s) was removed by column chromatography (silica gel, hexane, butch) and purification was performed by column chromatography (silica gel, hexane: methylene chloride = 10:1, Rf = 0.38). The resultant solid substance was dissolved in hot benzene and reprecipitated from hexane to obtain a white solid substance (3.3 g, 77%). 1H-NMR(400MHz,CDCl3)delta7.64-7.60(m,6H), 7.42-7.35(m,9H); 13C-NMR(99.5MHz,CDCl3)delta138.1,132.1, 129.5, 128.6, 123.1., 122.4, 101.1, 83.3; M.S.(70eV,EI)m/z=482(M+); mp186.8-187.3C
The synthetic route of 108-70-3 has been constantly updated, and we look forward to future research findings.
Reference:
Patent; Hiroshima University; Nippon Kayaku Kabushiki Kaisha; EP2361915; (2011); A1;,
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