反应详情

温度

90 °C

A reaction flask was equipped with a reflux condenser, agitator, addition funnel, nitrogen source and heating bath. The tris(6-carboxy-2-pyridyl)phosphine oxide sodium salt (310 mg, 0.65 mmol, MW 479) from Example 11 was dissolved warm demineralized water (10 mL) and the resultant solution was filtered and charged to reaction flask. Gadolinium (III) acetate (250 mg, 0.62 mmol, MW 406 for tetrahydrate) 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 100 mg of white solids (367 mg theoretical yield for anhydrous complex), and which had the following structural formula: ##STR15##

1. customA reaction flask was equipped with a reflux condenser
2. additionagitator, addition funnel, nitrogen source
3. temperatureheating bath
4. filtrationthe resultant solution was filtered
5. additioncharged to reaction flask
6. filtrationthe resultant solution was filtered
7. additioncharged to the addition funnel
8. additionthe gadolinium acetate solution was added dropwise with agitation over 30 min
9. additionOnce the addition
10. temperaturethe reaction was cooled to ambient temperature
11. customthe white solids were isolated by filtration
12. washwashed with demineralized water
13. customThe solids were dried in vacuo