1,3,5-Triazine, 2,4,6-tris(4-fluorophenyl)- synthesis

Yield: 45%

Reaction Conditions:

with iron(III) chloride;ammonium iodide in toluene at 130; for 15 h;Sealed tube;

Steps:

16 Example 16
The specific experimental operation for the synthesis of 2p is as follows: Weigh out 67 mg (0.5 mmol) of 4-fluorobenzaldehyde, 72.5 mg (0.5 mmol) of ammonium iodide, and 16.25 mg (0.1 mmol) of anhydrous ferric chloride in a 25 mL seal with a stir bar. In the tube, and add 2 mL of toluene. The reaction tube was sealed and placed in an oil bath at 130°C to heat and react for 15 hours under magnetic stirring to stop the reaction. The cooled reaction solution was washed with 6 mL of saturated NaCl solution, and then EtOAc (10 mL×3) was added to extract the reaction solution. The supernatant was collected and dried with anhydrous sodium sulfate to remove the water. Put the resulting mixture on a rotary evaporator and spin dry, add 4mL CH2Cl2, add silica gel powder, mix the sample evenly, load it into a filled silica gel column chromatography for separation and purification to obtain white 2,4,6-tris(4-fluorophenyl)- 1,3,5-triazine solid 81.67mg, the yield is 45%.

References:

Yuanjiang Hualong Catalysis Technology Co., Ltd.;Liu Qiang;Xiao Jiang;Guo Xin;Guo Cancheng CN111454226, 2020, A Location in patent:Paragraph 0161-0164