For complexing with Ce (III), two solutions 0.434 g of Ce(NO3)3.6H2O dissolved in 10 ml ethanol and 0.554 g of Schiff base dissolved in 10 ml ethanol were mixed in a round bottom flask
and then refluxed at 90AdegC for 8 h on a hot plate/magnetic stirrer with constant stirring using water condenser.
In a general experiment, 0.258 g (1 mmol) of compound 1b was dissolved in dichloromethane and mixed with 1 mmol of compound 2a-f in a round bottom flask
. After five minutes, a solution of 0.161 g (1 mmol) 3c, dissolved in 1 ml of dichloromethane was introduced in it by a pipette.
In a 250 [cm.sup.3] three-necked round bottom flask
10 g (0.0375 moles) EBUII and the appropriate amount of propylene carbonate (PC, pure, Fluka, Switzerland) were placed to reach the molar ratio of reagents of 1 : 6, 1 : 12, or 1:18 and 0.62 g potassium carbonate (16.6 g/mole EBU, 0.12 mole/mole EBU) was added.
The upper oily layer was transferred again to the round bottom flask
and 2g of NaOH and 20g of additional methanol was added to it.
0.9 mmol of diacid chloride was dissolved in THF at 0-5AdegC in a two-necked round bottom flask
fitted with reflux condenser and magnetic stirrer under inert environment.
To a 25 mL three-neck round bottom flask
equipped with a part flow arrangement and condenser under nitrogen.
2,4-Dihydroxyacetophenone (1.9 mmol, 1) was solubilized in 20 mL methanol and was taken in a 100 mL round bottom flask
. Equimolar quantity of hydrated hydrazine (1.9 mmol, 80 %, 2) along with two drops of glacial CH3COOH was added to the reaction mixture which was stirred for 3-4 hours till completion of reaction monitored by the TLC.
The PCII solution was put into a three-necked round bottom flask
with a stirrer, while the temperature was controlled at 18-25[degrees]C.
2-hydroxy acetophenone (1 mmol) was mixed with ethanolic KOH (40%, 2.0 mL) in a round bottom flask
and stirred for 20 mins at 25 degC.
In a 10 mL round bottom flask
furnished with magnetic stir bar was charged with tris (bipyridine) ruthenium (II) dichloride (1mol %) respective tetrahydroisoquinolines 1 and 1a (0.11 mm, 1 equiv.
A mixture of 1,10-phenenthroline 1 (5 g, 25.5 mmol) of and potassium bromide (5 g, 42 mmol) were taken in 100 mL round bottom flask
kept under ice bath than the a mixture of 50 mL of concentrated sulfuric acid and 25 mL nitric acid was added slowly with stirring at 0C and the reaction mixture was refluxed for 3 hrs.
A mixture of 4-methoxybenzyl bromide (Aldrich USA, 4.0g, 0.0199 mol), dry toluene (50 ml), triphenyl phosphine (Aldrich, 5.21 g, 0.0199 mol) in a round bottom flask
was refluxed under nitrogen for 24 hours.