Process for preparation of macrocyclic chelants and the chelates

Organic compounds -- part of the class 532-570 series – Organic compounds – Unsubstituted hydrocarbyl chain between the ring and the -c-...

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540472, 540465, 424 9363, C07D48722, A61B 5055

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active

060463244

ABSTRACT:
A process for the preparation of complexes of macrocyclic chelants with paramagnetic metal trivalent ions of formula (XII) ##STR1## wherein R.sub.1, R.sub.2 and Me.sup.3+ are as described in the following, comprising: a) reaction of 1,4,7,10-tetraazacyclododecane with triethyl orthoformate to give 5H,9bH-2a,4a,7,9a-octahydrotetraazacycloocta[cd]pentalene; b) carboxymethylation reaction in water; c) hydrolysis reaction in basic conditions; d) alkylation according to known methods with an epoxide in water; e) complexation according to known methods carried out in water by addition of a paramagnetic metal salt; f) purification by diafiltration, final desalting of the aqueous solution on ion exchange resins and g) crystallization or recovery.

REFERENCES:
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patent: 5747000 (1998-05-01), Platzek et al.
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Dischino et al Inorg. Chem. 1991, 30, pp. 1265-1269 Synthesis of Gadolinium (+)-10-(1-Hydroxypropan-2-yl)-1,4,7,10-tetraazacyclododecane-1,4,7-triyltr iacetate etc.
Weisman et al Tetrahedron Letters vol. 21, 1980 pp. 3635-3638.

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