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2) Synthesis of 2,4,6-tricyano-1,3,5-trimethylbenzene (TCM) CuCN (220g, 243 mmol) and pyridine (146.7g, 1.85 mol) were added to a high pressure reaction vessel, and well mixed, and then 2,4,6-tribromo-1,3,5-trimethylbenzene(25g, 75.8mmol) was added thereto. The reaction mixture was reacted at 205 0 for 2 hours. Cu therein was excluded with excessive methylene diamine, and then filtered by MC. Water in the reaction mixture was eliminated over MgSO4, and then solvent therein was evaporated in vacuum. The residue was absorbed to silica gel column and separated with a tube chromatography (Hx: MC = 3:1) to obtain white solid [yield: 6g (40.59%)].
In N,N-dimethyl-formamide; at 150 - 160℃; for 8.0h;Reflux;
To a solution of CuCN (5.0 g, 56.0 mmol) in 40.0 mL of DMF was added 2,4,6-dibromomesitylene (4.0 g, 30.0 mmol) and the resultant mixture was heated at reflux (150-160 C) for 8 h. Subsequently, the reaction mixture was cooled to room temperature and a solution of FeCl3 (24.0 g in 32.0 mL of 2.4 N HCl) was added. The mixture was heated at 78-80 C for 20 min and then cooled. The organic matter was extracted with chloroform, washed with water, dried over anhydrous Na2SO4 and the solvent removed in vacuo. The residue was subjected to column chromatography (10% ethyl acetate/hexane) to obtain 1.0 g (46%) of 2,4,6-Tricyanomesitylene as colourless crystalline material, mp 178-179 C (lit 180 C), 1H NMR (CDCl3, 400 MHz) 2.82 (s, 9H) ppm; 13C NMR (CDCl3, 100 MHz) δ 150.0, 114.4, 114.3, 20.8 ppm.
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