The preparation of proligands HL1 –HL8 was carried out with slight modifications
of the literature method.32 (link),33 (link) In the first step,
the corresponding aldehyde (1 mmol) and sodium bisulfide (10 mmol)
were stirred in water at 100 °C for 1 h. Then, o-phenylenediamine (1 mmol) was dissolved in EtOH and added to the
reaction mixture that was heated overnight at 80 °C. The corresponding
2-(aryl)benzimidazoleA1 –A8 (Scheme 2 ) were filtered and
washed with water and hexane. In the second step, the corresponding
2-(aryl)benzimidazole (0.5 mmol) and 4-(trifluoromethyl)benzyl bromide
or iodomethane (0.6 mmol) and Cs2CO3 (1 mmol)
were stirred in acetonitrile at 45 °C for 24 h. The solvent was
removed under reduced pressure, and dichloromethane was added and
extracted with water (3 × 30 mL). The organic phase was dried,
and a pure white solid was obtained.
of the literature method.32 (link),33 (link) In the first step,
the corresponding aldehyde (1 mmol) and sodium bisulfide (10 mmol)
were stirred in water at 100 °C for 1 h. Then, o-phenylenediamine (1 mmol) was dissolved in EtOH and added to the
reaction mixture that was heated overnight at 80 °C. The corresponding
2-(aryl)benzimidazole
washed with water and hexane. In the second step, the corresponding
2-(aryl)benzimidazole (0.5 mmol) and 4-(trifluoromethyl)benzyl bromide
or iodomethane (0.6 mmol) and Cs2CO3 (1 mmol)
were stirred in acetonitrile at 45 °C for 24 h. The solvent was
removed under reduced pressure, and dichloromethane was added and
extracted with water (3 × 30 mL). The organic phase was dried,
and a pure white solid was obtained.
Free full text: Click here
