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2.5
Synthesis of Heterometallic Diethanolaminate Alkoxide Derivatives
Similar to homometallic glycolates of alkaline earth metals (M D Mg, Ca, Sr, Ba),
diethanolaminates also can be prepared by dissolution of the metals or by reactions of
their isopropoxides with diethanolamine (Eqs 3.97 and 3.98):
toluene
! Mf OC 2 H 4 HOC 2 H 4 NHg 2 #CH 2 "
M C 2HN C 2 H 4 OH 2
3 . 97
M OPr i 2 C2HN C 2 H 4 OH 2 ! Mf OC 2 H 4 HOC 2 H 4 NHg 2 #C2Pr i OH "
A 0 Colourless, insoluble solid
3 . 98
The colourless solids ( A 0 ) differ from ( A ) (Section 2.4) in being insoluble in organic
solvents. However, on being reacted with Al OPr i 3 , A 0 also yields 171 ahetero-
bimetallic diethanolaminate product ( B 0 ) which is a colourless, soluble, monomeric
non-volatile solid (Eq. 3.99).
benzene
!fAl OPr i 2 g 2 Mf OC 2 H 4 2 NHg 2
B 0
A 0 C 2Al OPr i 3
C 2Pr i OH "
3 . 99
Other colourless, soluble monomeric solids ( C 0 )and( D 0 ), with the compositions
MfAl OPr i 2 gf OC 2 H 4 2 NHg 2 and MfAl OC 2 H 4 NHC 2 H 4 O 2 g 2 , respectively, can also
be synthesized by reactions similar to those of Eqs (3.93) and (3.94).
Heterobimetallic diethanolaminate derivatives of a number of other metals have also
been synthesized 172
by similar reactions (Eqs 3.100 - 3.102):
M OPr i 3 C 2HN C 2 H 4 OH 2
benzene
! Mf OC 2 H 4 HOC 2 H 4 NHgf OC 2 H 4 2 NHg#
( E ), ( F )
C 3Pr i OH "
3 . 100
where M D Al, Sb.
Ti OPr i 4 C 3HN C 2 H 4 OH 2
benzene
! Tif OC 2 H 4 2 NHgf HOC 2 H 4 OC 2 H 4 NHg 2 #
( G )
C 4Pr i OH "
3 . 101
M 0 OPr i 4 . Pr i OH C 3HN C 2 H 4 OH 2
benzene
! M 0 f OC 2 H 4 2 NHgf HOC 2 H 4 OC 2 H 4 NHg 2 #
( H ), ( I )
C 5Pr i OH "
3 . 102
where M 0 D Zr, Sn( IV ).
The products ( E ), ( F ), ( G ), ( H ), and ( I ) are colourless, insoluble nonvolatile solids,
which can be converted into heterobimetallic soluble monomeric products by reactions
represented Eqs (3.103) - (3.105):
benzene
!fNb OPr i 4 gfAl[ OC 2 H 4 2 NH] 2 gCPr i OH "
E CNb OPr i 5
3 . 103
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