Acetic acid, gadolinium(3+) salt (3:1) → HCID 86753609, compound

Participants

Reaction Conditions

Reaction Steps

A reaction flask was equipped with a reflux condenser, agitator, addition funnel, nitrogen source and heating bath. The tris(6-carboxy-2-pyridyl)phosphine sodium salt (310 mg, 0.67 mmol, MW 463) from Example 9 was dissolved warm demineralized water (10 mL) and the resultant solution was filtered and charged to reaction flask. Gadolinium (III) acetate (260 mg, 0.64 mmol, MW 406 for tetrahydrate, 1 equiv) was dissolved in warm demineralized water (10 mL) and the resultant solution was filtered and charged to the addition funnel. The bath was heated to 90° C. and the gadolinium acetate solution was added dropwise with agitation over 30 min. Once the addition was complete, the reaction was cooled to ambient temperature and the white solids were isolated by filtration and washed with demineralized water. The solids were dried in vacuo to afford 130 mg of white solids (369 mg theoretical yield for anhydrous complex, 93% by HPLC area%/o), and having the structural formula shown below: ##STR14##

Provenance & Evidence