Synthesis evidence

Synthesis, conductivity, and electromagnetic wave absorption properties of chiral poly Schiff bases and their silver complexes

Li H., Liu C., Dai B. et al. · Journal of Applied Polymer Science · 2015 · 42498

9 structured synthesis routes

Completeness describes how fully the route could be reconstructed from the main article and supporting information.

Complete recipeSource: Main

Route 1: Other

3 · Experimental - Synthesis of Chiral Poly Schiff Bases Silver Complexes · Figure 1

Metal precursorsAgNO3 (2.04 g; 12 mmol).
Linker precursorsL-lysine (1.46 g, 10 mmol) and p-benzoquinone (10 mmol).
SolventsAbsolute ethanol: 40 mL for lysine/KOH solution plus 30 mL for dicarbonyl solution.
AdditivesKOH (0.56 g, 10 mmol); zinc chloride (0.05 g) catalyst.
AtmosphereNitrogen.
Temperature80
Time12 total: 6 h before AgNO3 addition plus 6 h after AgNO3 addition.
Work-upPrecipitate collected by vacuum filtration and washed with ethanol three times.
ActivationDried in a vacuum desiccator.
Scalability contextBatch scale: 10 mmol lysine, 10 mmol dicarbonyl compound, 12 mmol AgNO3 in a 250 mL round-bottom flask.
Show 6 structured reagent records
RoleReagentAmount / concentrationSource
LinkerL-lysine1.46 g; 10 mmol3 · Experimental - Synthesis of Chiral Poly Schiff Bases Silver Complexes · Figure 1
BaseKOH0.56 g; 10 mmol3 · Experimental - Synthesis of Chiral Poly Schiff Bases Silver Complexes · Figure 1
Solventabsolute ethanol40 mL + 30 mL3 · Experimental - Synthesis of Chiral Poly Schiff Bases Silver Complexes · Figure 1
Linkerp-benzoquinone10 mmol3 · Experimental - Synthesis of Chiral Poly Schiff Bases Silver Complexes · Figure 1
Additivezinc chloride0.05 g3 · Experimental - Synthesis of Chiral Poly Schiff Bases Silver Complexes · Figure 1
Metal SourceAgNO32.04 g; 12 mmol3 · Experimental - Synthesis of Chiral Poly Schiff Bases Silver Complexes · Figure 1
Complete recipeSource: Main

Route 2: Other

3 · Experimental - Synthesis of Chiral Poly Schiff Bases Silver Complexes · Figure 1

Metal precursorsAgNO3 (2.04 g; 12 mmol).
Linker precursorsDL-lysine (1.46 g, 10 mmol) and p-benzoquinone (10 mmol).
SolventsAbsolute ethanol: 40 mL for lysine/KOH solution plus 30 mL for dicarbonyl solution.
AdditivesKOH (0.56 g, 10 mmol); zinc chloride (0.05 g) catalyst.
AtmosphereNitrogen.
Temperature80
Time12 total: 6 h before AgNO3 addition plus 6 h after AgNO3 addition.
Work-upPrecipitate collected by vacuum filtration and washed with ethanol three times.
ActivationDried in a vacuum desiccator.
Scalability contextBatch scale: 10 mmol lysine, 10 mmol dicarbonyl compound, 12 mmol AgNO3 in a 250 mL round-bottom flask.
Show 6 structured reagent records
RoleReagentAmount / concentrationSource
LinkerDL-lysine1.46 g; 10 mmol3 · Experimental - Synthesis of Chiral Poly Schiff Bases Silver Complexes · Figure 1
BaseKOH0.56 g; 10 mmol3 · Experimental - Synthesis of Chiral Poly Schiff Bases Silver Complexes · Figure 1
Solventabsolute ethanol40 mL + 30 mL3 · Experimental - Synthesis of Chiral Poly Schiff Bases Silver Complexes · Figure 1
Linkerp-benzoquinone10 mmol3 · Experimental - Synthesis of Chiral Poly Schiff Bases Silver Complexes · Figure 1
Additivezinc chloride0.05 g3 · Experimental - Synthesis of Chiral Poly Schiff Bases Silver Complexes · Figure 1
Metal SourceAgNO32.04 g; 12 mmol3 · Experimental - Synthesis of Chiral Poly Schiff Bases Silver Complexes · Figure 1
Complete recipeSource: Main

Route 3: Other

3 · Experimental - Synthesis of Chiral Poly Schiff Bases Silver Complexes · Figure 1

Metal precursorsAgNO3 (2.04 g; 12 mmol).
Linker precursorsL-lysine (1.46 g, 10 mmol) and 1,4-naphthoquinone (10 mmol).
SolventsAbsolute ethanol: 40 mL for lysine/KOH solution plus 30 mL for dicarbonyl solution.
AdditivesKOH (0.56 g, 10 mmol); zinc chloride (0.05 g) catalyst.
AtmosphereNitrogen.
Temperature80
Time12 total: 6 h before AgNO3 addition plus 6 h after AgNO3 addition.
Work-upPrecipitate collected by vacuum filtration and washed with ethanol three times.
ActivationDried in a vacuum desiccator.
Scalability contextBatch scale: 10 mmol lysine, 10 mmol dicarbonyl compound, 12 mmol AgNO3 in a 250 mL round-bottom flask.
Show 6 structured reagent records
RoleReagentAmount / concentrationSource
LinkerL-lysine1.46 g; 10 mmol3 · Experimental - Synthesis of Chiral Poly Schiff Bases Silver Complexes · Figure 1
BaseKOH0.56 g; 10 mmol3 · Experimental - Synthesis of Chiral Poly Schiff Bases Silver Complexes · Figure 1
Solventabsolute ethanol40 mL + 30 mL3 · Experimental - Synthesis of Chiral Poly Schiff Bases Silver Complexes · Figure 1
Linker1,4-naphthoquinone10 mmol3 · Experimental - Synthesis of Chiral Poly Schiff Bases Silver Complexes · Figure 1
Additivezinc chloride0.05 g3 · Experimental - Synthesis of Chiral Poly Schiff Bases Silver Complexes · Figure 1
Metal SourceAgNO32.04 g; 12 mmol3 · Experimental - Synthesis of Chiral Poly Schiff Bases Silver Complexes · Figure 1
Complete recipeSource: Main

Route 4: Other

3 · Experimental - Synthesis of Chiral Poly Schiff Bases Silver Complexes · Figure 1

Metal precursorsAgNO3 (2.04 g; 12 mmol).
Linker precursorsL-lysine (1.46 g, 10 mmol) and dibenzoyl (10 mmol).
SolventsAbsolute ethanol: 40 mL for lysine/KOH solution plus 30 mL for dicarbonyl solution.
AdditivesKOH (0.56 g, 10 mmol); zinc chloride (0.05 g) catalyst.
AtmosphereNitrogen.
Temperature80
Time12 total: 6 h before AgNO3 addition plus 6 h after AgNO3 addition.
Work-upPrecipitate collected by vacuum filtration and washed with ethanol three times.
ActivationDried in a vacuum desiccator.
Scalability contextBatch scale: 10 mmol lysine, 10 mmol dicarbonyl compound, 12 mmol AgNO3 in a 250 mL round-bottom flask.
Show 6 structured reagent records
RoleReagentAmount / concentrationSource
LinkerL-lysine1.46 g; 10 mmol3 · Experimental - Synthesis of Chiral Poly Schiff Bases Silver Complexes · Figure 1
BaseKOH0.56 g; 10 mmol3 · Experimental - Synthesis of Chiral Poly Schiff Bases Silver Complexes · Figure 1
Solventabsolute ethanol40 mL + 30 mL3 · Experimental - Synthesis of Chiral Poly Schiff Bases Silver Complexes · Figure 1
Linkerdibenzoyl10 mmol3 · Experimental - Synthesis of Chiral Poly Schiff Bases Silver Complexes · Figure 1
Additivezinc chloride0.05 g3 · Experimental - Synthesis of Chiral Poly Schiff Bases Silver Complexes · Figure 1
Metal SourceAgNO32.04 g; 12 mmol3 · Experimental - Synthesis of Chiral Poly Schiff Bases Silver Complexes · Figure 1
Complete recipeSource: Main

Route 5: Other

3 · Experimental - Synthesis of Chiral Poly Schiff Bases Silver Complexes · Figure 1

Metal precursorsAgNO3 (2.04 g; 12 mmol).
Linker precursorsL-lysine (1.46 g, 10 mmol) and 2,3-butanedione (10 mmol).
SolventsAbsolute ethanol: 40 mL for lysine/KOH solution plus 30 mL for dicarbonyl solution.
AdditivesKOH (0.56 g, 10 mmol); zinc chloride (0.05 g) catalyst.
AtmosphereNitrogen.
Temperature80
Time12 total: 6 h before AgNO3 addition plus 6 h after AgNO3 addition.
Work-upPrecipitate collected by vacuum filtration and washed with ethanol three times.
ActivationDried in a vacuum desiccator.
Scalability contextBatch scale: 10 mmol lysine, 10 mmol dicarbonyl compound, 12 mmol AgNO3 in a 250 mL round-bottom flask.
Show 6 structured reagent records
RoleReagentAmount / concentrationSource
LinkerL-lysine1.46 g; 10 mmol3 · Experimental - Synthesis of Chiral Poly Schiff Bases Silver Complexes · Figure 1
BaseKOH0.56 g; 10 mmol3 · Experimental - Synthesis of Chiral Poly Schiff Bases Silver Complexes · Figure 1
Solventabsolute ethanol40 mL + 30 mL3 · Experimental - Synthesis of Chiral Poly Schiff Bases Silver Complexes · Figure 1
Linker2,3-butanedione10 mmol3 · Experimental - Synthesis of Chiral Poly Schiff Bases Silver Complexes · Figure 1
Additivezinc chloride0.05 g3 · Experimental - Synthesis of Chiral Poly Schiff Bases Silver Complexes · Figure 1
Metal SourceAgNO32.04 g; 12 mmol3 · Experimental - Synthesis of Chiral Poly Schiff Bases Silver Complexes · Figure 1
Complete recipeSource: Main

Route 6: Other

2 · Experimental - Synthesis of the Chiral Poly Schiff Bases · Figure 1

Metal precursorsKOH used to form potassium carboxylate salt; no transition metal precursor.
Linker precursorsL-lysine (1.46 g, 10 mmol) and p-benzoquinone (10 mmol).
SolventsAbsolute ethanol: 40 mL for L-lysine/KOH solution plus 30 mL for dicarbonyl solution.
AdditivesKOH (0.56 g, 10 mmol); a few grains of zinc chloride catalyst.
AtmosphereNitrogen.
Temperature80
Time12
Work-upPrecipitate collected by vacuum filtration and washed with absolute ethanol three times.
ActivationDried in a vacuum desiccator.
Scalability contextBatch scale: 10 mmol L-lysine and 10 mmol dicarbonyl compound in a 250 mL round-bottom flask.
Show 5 structured reagent records
RoleReagentAmount / concentrationSource
LinkerL-lysine1.46 g; 10 mmol2 · Experimental - Synthesis of the Chiral Poly Schiff Bases · Figure 1
BaseKOH0.56 g; 10 mmol2 · Experimental - Synthesis of the Chiral Poly Schiff Bases · Figure 1
Solventabsolute ethanol40 mL + 30 mL2 · Experimental - Synthesis of the Chiral Poly Schiff Bases · Figure 1
Linkerp-benzoquinone10 mmol2 · Experimental - Synthesis of the Chiral Poly Schiff Bases · Figure 1
Additivezinc chloridea few grains2 · Experimental - Synthesis of the Chiral Poly Schiff Bases · Figure 1
Complete recipeSource: Main

Route 7: Other

2 · Experimental - Synthesis of the Chiral Poly Schiff Bases · Figure 1

Metal precursorsKOH used to form potassium carboxylate salt; no transition metal precursor.
Linker precursorsL-lysine (1.46 g, 10 mmol) and 1,4-naphthoquinone (10 mmol).
SolventsAbsolute ethanol: 40 mL for L-lysine/KOH solution plus 30 mL for dicarbonyl solution.
AdditivesKOH (0.56 g, 10 mmol); a few grains of zinc chloride catalyst.
AtmosphereNitrogen.
Temperature80
Time12
Work-upPrecipitate collected by vacuum filtration and washed with absolute ethanol three times.
ActivationDried in a vacuum desiccator.
Scalability contextBatch scale: 10 mmol L-lysine and 10 mmol dicarbonyl compound in a 250 mL round-bottom flask.
Show 5 structured reagent records
RoleReagentAmount / concentrationSource
LinkerL-lysine1.46 g; 10 mmol2 · Experimental - Synthesis of the Chiral Poly Schiff Bases · Figure 1
BaseKOH0.56 g; 10 mmol2 · Experimental - Synthesis of the Chiral Poly Schiff Bases · Figure 1
Solventabsolute ethanol40 mL + 30 mL2 · Experimental - Synthesis of the Chiral Poly Schiff Bases · Figure 1
Linker1,4-naphthoquinone10 mmol2 · Experimental - Synthesis of the Chiral Poly Schiff Bases · Figure 1
Additivezinc chloridea few grains2 · Experimental - Synthesis of the Chiral Poly Schiff Bases · Figure 1
Complete recipeSource: Main

Route 8: Other

2 · Experimental - Synthesis of the Chiral Poly Schiff Bases · Figure 1

Metal precursorsKOH used to form potassium carboxylate salt; no transition metal precursor.
Linker precursorsL-lysine (1.46 g, 10 mmol) and dibenzoyl (10 mmol).
SolventsAbsolute ethanol: 40 mL for L-lysine/KOH solution plus 30 mL for dicarbonyl solution.
AdditivesKOH (0.56 g, 10 mmol); a few grains of zinc chloride catalyst.
AtmosphereNitrogen.
Temperature80
Time12
Work-upPrecipitate collected by vacuum filtration and washed with absolute ethanol three times.
ActivationDried in a vacuum desiccator.
Scalability contextBatch scale: 10 mmol L-lysine and 10 mmol dicarbonyl compound in a 250 mL round-bottom flask.
Show 5 structured reagent records
RoleReagentAmount / concentrationSource
LinkerL-lysine1.46 g; 10 mmol2 · Experimental - Synthesis of the Chiral Poly Schiff Bases · Figure 1
BaseKOH0.56 g; 10 mmol2 · Experimental - Synthesis of the Chiral Poly Schiff Bases · Figure 1
Solventabsolute ethanol40 mL + 30 mL2 · Experimental - Synthesis of the Chiral Poly Schiff Bases · Figure 1
Linkerdibenzoyl10 mmol2 · Experimental - Synthesis of the Chiral Poly Schiff Bases · Figure 1
Additivezinc chloridea few grains2 · Experimental - Synthesis of the Chiral Poly Schiff Bases · Figure 1
Complete recipeSource: Main

Route 9: Other

2 · Experimental - Synthesis of the Chiral Poly Schiff Bases · Figure 1

Metal precursorsKOH used to form potassium carboxylate salt; no transition metal precursor.
Linker precursorsL-lysine (1.46 g, 10 mmol) and 2,3-butanedione (10 mmol).
SolventsAbsolute ethanol: 40 mL for L-lysine/KOH solution plus 30 mL for dicarbonyl solution.
AdditivesKOH (0.56 g, 10 mmol); a few grains of zinc chloride catalyst.
AtmosphereNitrogen.
Temperature80
Time12
Work-upPrecipitate collected by vacuum filtration and washed with absolute ethanol three times.
ActivationDried in a vacuum desiccator.
Scalability contextBatch scale: 10 mmol L-lysine and 10 mmol dicarbonyl compound in a 250 mL round-bottom flask.
Show 5 structured reagent records
RoleReagentAmount / concentrationSource
LinkerL-lysine1.46 g; 10 mmol2 · Experimental - Synthesis of the Chiral Poly Schiff Bases · Figure 1
BaseKOH0.56 g; 10 mmol2 · Experimental - Synthesis of the Chiral Poly Schiff Bases · Figure 1
Solventabsolute ethanol40 mL + 30 mL2 · Experimental - Synthesis of the Chiral Poly Schiff Bases · Figure 1
Linker2,3-butanedione10 mmol2 · Experimental - Synthesis of the Chiral Poly Schiff Bases · Figure 1
Additivezinc chloridea few grains2 · Experimental - Synthesis of the Chiral Poly Schiff Bases · Figure 1