N-[1,1'-biphenyl]-4-yl-aminophenathrene synthesis
- Product Name:N-[1,1'-biphenyl]-4-yl-aminophenathrene
- CAS Number:443965-64-8
- Molecular formula:C26H19N
- Molecular Weight:345.44
Yield:443965-64-8 86.55%
Reaction Conditions:
with tris-(dibenzylideneacetone)dipalladium(0);tri-tert-butyl phosphine;sodium tertiary butoxide in toluene at 115; for 12 h;Inert atmosphere;
Steps:
4
After dissolving raw material A (40.00 mmol) and raw material B (40.00 mmol) in toluene, under N2 atmosphere, Pd2(dba)3(0.40 mmol), P(t-Bu)3(2.00 mmol) and t- BuONa (80.00 mmol) was heated to 115 °C and stirred for 12 h. After the reaction was completed, diatomaceous earth was used for suction filtration while hot to remove salt and catalyst. After the filtrate was cooled to room temperature, distilled water was added to the filtrate for washing. The organic phase was retained, the aqueous phase was extracted with ethyl acetate, then the combined organic layers were dried using magnesium sulfate, and the solvent was removed using a rotary evaporator, and finally mixed with dichloromethane and petroleum ether (V:V=1:16) The mixture was used as an eluent, and the remaining material was purified by column chromatography to obtain the compound represented by Intermediate 1 (11.95 g, yield: 86.55%).
References:
CN114853701,2022,A Location in patent:Paragraph 0096-0099
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