Molecules 2003, 8
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Table 4 . Modifications effected in the domestic microwave oven
Domestic Microwave oven
1. Rotating plate
Modified Microwave oven
1. Removed and magnetic stirrer is fitted
2. Provision made for inserting a reflux
condenser (B19 size)
2. Leak proof top cover
3. Microwave source (both from the
side and top)
3. Microwave source from one side only.
General experimental procedure for Michael addition reaction using Al – Complex 3
In an oven dried side arm flask closed with a septum and containing LiAlH4 (0.038 g, 1 mmol) in
dry THF (2 mL) was added 3 (0.237 g, 1 mmol) in dry THF (3 mL) at room temperature. The resulting
mixture was stirred for one hour. To the stirred solution 2-cyclohexenone (0.490g, 5 mmol) and diethyl
malonate, (0.800 g, 5 mmol) were added and the mixture was irradiated in a microwave oven for the
stipulated period of time. The reaction was quenched with dil. HCl and extracted with ethyl acetate
(3x10 mL). The organic layer was washed with water, followed by saturated. NaHCO3 solution. The
combined organic layers were dried over anhydrous Na2SO4 and the solvent were removed under
o
reduced pressure to yield the product. (1.1 g. 90 % yield, [ o]=-2.3 78 % ee ). All the products were
a
D
identified and characterized by their H and 13C-NMR spectral data and found identical with the
1
literature reported values [11].
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