Titanium isopropoxide → HCID 131730574, compound

Temperature

100 °C

A solution of 4-nitrocatechol (10 g, 64.5 mmol) and toluene (220 ml) was dehydrated by distilling 20 mL of the solution. Thereafter, 9.15 g (32.2 mmol) of titanium(IV) isopropoxide (TTIP) 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 (4-nitrocatechol-titanium complex) was brown in color. The yield amount was 11.0 g (31.1 mmol), and the yield percentage was 97%. 3.54 g of 4-nitrocatechol-titanium complex was dissolved into 100 mL of 1:4 acetylacetone/toluene to produce a coating liquid.

1. distillationby distilling 20 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. dissolution3.54 g of 4-nitrocatechol-titanium complex was dissolved into 100 mL of 1:4 acetylacetone/toluene
11. customto produce a coating liquid

ORD record

ord-54238745f56e444097dbb8d77e82292f

Source dataset

uspto-grants-2013_05

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US08445118B2