bis{4-[bis(4-tert-butylphenyl)amine]phenyl} sulfone synthesis

Yield:1396165-17-5 77%

Reaction Conditions:

Stage #1: bis(4-tert-butylphenyl)aminewith sodium hydride in N,N-dimethyl-formamide at 20; for 0.5 h;
Stage #2: bis(p-fluorophenyl)sulfone in N,N-dimethyl-formamide at 100; for 1 h;

Steps:

1 synthesis of compound 3

Bis (4-tert-butylphenyl) amine (4.22 g, 15 mmol) was added to a solution of sodium hydride (0.72 g, 30 mmol) in dehydrated N, N-dimethylformamide (DMF: 30 mL). The resulting solution was stirred at room temperature for 30 minutes, and a solution of bis (p-fluorophenyl) sulfone (1.91 g, 7.5 mmol) in dehydrated DMF (30 mL) was added. Thereafter, the mixture was further stirred at 100 DEG C for 1 hour, cooled, and then injected into 400 mL of water. The resulting white solid was filtered and dried, and the obtained crude product was further recrystallized from chloroform and ethyl ether to obtain 4.5 g of white crystals (yield: 77%).

References:

KR2015/16242,2015,A Location in patent:Paragraph 0242-0244