Titanium isopropoxide → HCID 131730572, compound

HRID 2093255Notes

Reaction equation

HRID 2093255 reaction equation
[OH:1][C:2]1[CH:3]=[C:4]([CH:7]=[CH:8][C:9]=1O)[C:5]#[N:6].CC(C)[O-:13].[Ti+4:15].CC(C)[O-:18].CC(C)[O-].CC(C)[O-]>C1(C)C=CC=CC=1>[C:5]([C:4]1[CH:7]=[CH:8][CH:9]=[C:2]([O-:1])[C:3]=1[O-:13])#[N:6].[Ti+4:15].[C:5]([C:4]1[CH:7]=[CH:8][CH:9]=[C:2]([O-:1])[C:3]=1[O-:18])#[N:6]

Participants

4

Reactant 2

HCID 11026Titanium isopropoxideHCID 870653,4-Dihydroxybenzonitrile

Product 1

HCID 131730572HCID 131730572, compound

Reagents, catalysts & solvents 1

HCID 1140TolueneSolvent

Conditions

Temperature
100 °C

Procedure

A solution of 3,4-dihydroxybenzonitrile (5.00 g, 37.0 mmol) and toluene (45 ml) was dehydrated by distilling 5 mL of the solution. Thereafter, 5.25 g (18.5 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 (3,4-dihydroxybenzonitrile-titanium complex) was brown in color. The yield amount was 5.80 g (18.5 mmol), and the yield percentage was 100%. 3.14 g of 3,4-dihydroxybenzonitrile-titanium complex was dissolved into 100 mL of ethanol to produce a coating liquid.

Workup

  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. dissolution3.14 g of 3,4-dihydroxybenzonitrile-titanium complex was dissolved into 100 mL of ethanol
  11. customto produce a coating liquid

Sources & evidence

ORD record
ord-5950ddba70544d319efae6c0e20de10d
Source dataset
uspto-grants-2013_05
Patent number
US08445118B2

Reaction notes

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