2,9-bis(4-methoxyphenyl)-1,10-phenanthroline synthesis
- Product Name:2,9-bis(4-methoxyphenyl)-1,10-phenanthroline
- CAS Number:89333-97-1
- Molecular formula:C26H20N2O2
- Molecular Weight:392.45
5720-07-0
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Yield:89333-97-1 96%
Reaction Conditions:
with tetrakis(triphenylphosphine) palladium(0);sodium carbonate in water;toluene at 80; for 16 h;Inert atmosphere;
Steps:
Synthesis of 4
To a solution of compound 1 (0.2 g, 0.8 mmol) and 19 (0.34 g, 2.2 mmol) in toluene (16 mL) was added a solution of Na2CO3 (1.7 g, 16 mmol) in water (8 mL). The two-phase mixture was degassed and then Pd(PPh3)4 (28 mg, 0.02 mmol) was rapidly added under a flow of argon. The mixture was heated at 80 °C with vigorous stirring for 16 h. It was then allowed to cool to room temperature and CH2Cl2 (90 mL) was added. The organic layer was washed with brine (20 mL), dried over Na2SO4 and then filtered. The resulting filtrate was concentrated in reduced pressure. The residue was purified by column chromatography (CHCl3/Hex = 6/1) to give the compound 4 (0.30 g, 96%).
References:
Kim, Nam-Kyun;Sogawa, Hiromitsu;Takata, Toshikazu [Tetrahedron Letters,2020,vol. 61,# 23,art. no. 151966] Location in patent:supporting information
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