10
A. DESAI AND D. RANA
Synthesis of calixsalen-type cavitands
General procedure
DCM (2 L) was added to a 5 L three-necked round bottom flask equipped with two
addition funnels. Solution of 5,50-methylene-bis-aldehydes (0.004 mol) in DCM (1 L) and
ethylenediamine (0.004 mol) in DCM (1 L) were added drop wise from addition funnels
over 10 h to the mechanically stirred DCM under N2 atmosphere. Bright yellow color
was developed gradually. TLC of reaction mixture showed very small amount of starting
material, non-polar product spot and many polar impurities. Solvent was removed under
vacuum. Reaction mixture was employed for column chromatography. Starting material
was eluted in DCM and pure yellow product was separated using DCM:methanol solvent
system (gradient), the polar impurities were retained in column.
Funding
We acknowledge research and consultancy cell, The M.S. University of Baroda for financial support,
and sophisticated analytical instrument facility, IIT Bombay as well as SIC Indore for recording
HRMS analysis.
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