Self-assembled Transition Metal Coordination Frameworks of ...

M p p p Ligands
HCl and the solid separated was filtered, washed well with distilled water and dried
carefully to get the buff coloured product. Yield: 80%, M.p. 197 °C.
LC], N/CH3 /‘‘S OH
Scheme 2.5. Reaction scheme of carboxymethyl N-methyl, N-phenyl
dithiocarbamate.
(ii) Preparation of N( 4)-methyl, N( 4) -phenyl 3-thiosemicarbazide
A solution of 17.700 g (0.073 mol) of carboxymethyl N-methyl, N-phenyl
dithiocarbamate in 20 ml 98% hydrazine hydrate and 10 ml distilled water was heated
on the rings of a steam bath at 85 °C. After 3 minutes crystals began to separate.
Heating was continued for additional 22 minutes. The crystals were collected by
filtration, washed well with distilled water and dried. This was then recrystallized
from a mixture of 2:1 v/v absolute ethanol: distilled water to get the stout colored
Q uf\, O
crystals of 4-methyl, 4-phenyl 3-thiosemicarbazide. Yield: 65%, M.p. 124 °C.
N/CH3 //O _ f CH3
"' CH2
8% H _