Catechol → Hafnium Catecholate

Temperature

100 °C

A solution of catechol (2.34 g, 2.12 mmol) and toluene (26 ml) was dehydrated by distilling 5 mL of the solution. Thereafter, 5.00 g (10.6 mmol) of hafnium(IV) butoxide was added to the solution while stirring. The mixed solution was refluxed for 1 hour, and then, while the distillation temperature was 100° C. or higher, distilled until the amount of the solution became half. After the distillation, solid content of the product was isolated by suction filtering using a membrane suction filter. The residual solid content was heated to 100° C. under vacuum using a vacuum dryer so that remaining volatile components were completely removed. The solid content (catechol-hafnium complex) was black in color. The yield amount was 4.18 g (10.6 mmol), and the yield percentage was 100%. Catechol-hafnium complex was dissolved into acetylacetone until saturated, and then filtered to be used as a coating liquid.

1. distillationby distilling 5 mL of the solution
2. temperatureThe mixed solution was refluxed for 1 hour
3. customwas 100° C.
4. distillationhigher, distilled until the amount of the solution
5. distillationAfter the distillation, solid content of the product
6. customwas isolated by suction
7. filtrationfiltering
8. filtrationfilter
9. customwere completely removed
10. dissolutionCatechol-hafnium complex was dissolved into acetylacetone until saturated, and
11. filtrationthen filtered

ORD record

ord-f6e37cf92c794dd1acb198848165c4e2

Source dataset

uspto-grants-2013_05

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US08445118B2