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With tri-tert-butyl phosphine; bis(dibenzylideneacetone)-palladium(0); sodium t-butanolate; In toluene; at 100℃; for 12h;Inert atmosphere; Reflux;
Nitrogen environment intermediates in the I-3 (20 g, 62. 1 mmol) of toluene 0. 2 L senses a rotation velocity of the disk to, herein chemical technology Shenzhen gre-a syn3 homolog (http://www. Gre-a syn3 homolog. Com /) yarn dibiphenyl-4-ylamine (20. 0 g, 62. 1 mmol), bis (dibenzylideneacetone) palladium (0) (0. 36 g, 0. 62 mmol), tris-tert butylphosphine (0. 63 g, 3. 11 mmol) and sodium tert-butoxide (7. 16 g, 74. 5 mmol) 100 °C and at sequentially in the reflux by heating at a 12. Complete after reaction solution at a water doesn't have any error frames, then dichloromethane (DCM) extraction of water to the MgSO4 anhydride after triggers number, filter and was, concentrating it under reduced pressure. Thus-obtained residue number 2 - 2 compound number 2 the forward separated into flash column chromatography (17. 5 g, 50percent) for obtained.
With bis(tri-t-butylphosphine)palladium(0); sodium t-butanolate; In 5,5-dimethyl-1,3-cyclohexadiene; for 3h;Inert atmosphere; Reflux;
To a 500 ml round bottom flask in a nitrogen atmosphereCompound 1-Bromobenzofuran (10.0 g, 40.65 mmol), Di ([1,1'-biphenyl] -4-yl) amine (14.35 g, 44.72 mmol)Was completely dissolved in 240 ml of xylene and then sodium tertbutoxide(sodium tertbutoxide) (5.08 g, 52.85 mol) was added,Bis (tri-tert-butylphosphine) palladium (0)(Bis(tri-tert-butylphosphine)palladium(0)) (0.21 g, 0.41 mmol) was added thereto and the mixture was heated with stirring for 3 hours.After the temperature was lowered to room temperature and the salts were removed by filtration, xylene was concentrated under reduced pressure and the residue was subjected to column chromatography using tetrahydrofuran: hexane = 1: 15 to prepare Compound 1 (12.84 g, yield 65percent)
With palladium diacetate; triphenylphosphine; sodium t-butanolate; In toluene; at 80℃; for 8h;Inert atmosphere;
Under argon atmosphere, 12.96 g (50 mmol) of <strong>[66127-01-3]3-bromophenanthroline</strong>, 16.07 g (50 mmol) of bis(4-biphenyl)amine, 9.61 g (100 mmol) of sodium tert-butoxide dissolved in 500 ml of dehydrated toluene, 0.22 g (1 mmol) of palladium acetate and 0.26 g (1 mmol) of triphenylphosphine were added under stirring, and the mixture was reacted at 80 C for 8 hours. after cooling, it was filtered through a Celite/silica gel funnel, and the filtrate was evaporated to remove organic solvent. the resulting residue was recrystallized from toluene and dried.22.23 g (44.5 mmol) of compound HT1 was obtained in a yield of 89%.
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