Synthesis evidence

Synthesis, characterization, electrical conductivity, and catalytic studies of some coordination polymers of salen-type schiff base

Pardhi A.V., Bansod A.D., Yaul A.R. et al. · Russian Journal of Coordination Chemistry/Koordinatsionnaya Khimiya · 2010 · 298-304

9 structured synthesis routes

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

Partial recipeSource: Main

Route 1: Other

300 · Experimental - Synthesis of polychelates

Metal precursorscadmium(II) chloride monohydrate; 1.00 mmol
Linker precursorsH2BNESAP; 1.00 mmol
SolventsDMF, minimum quantity 25-30 ml for each solution
Additivessodium acetate, 1 g
Atmosphereair/not specified
Temperaturehot conditions; sand bath; dried at 80
Time3-4
Work-upFiltered; washed thoroughly with hot water, DMF, ethanol and acetone; dried in an oven at 80 C.
Activationdried in an oven at 80 C
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
Metal Sourcecadmium(II) chloride monohydrate1.00 mmol300 · Experimental - Synthesis of polychelates
LinkerH2BNESAP1.00 mmol300 · Experimental - Synthesis of polychelates
SolventDMF25-30 ml minimum quantity for each solution300 · Experimental - Synthesis of polychelates
Basesodium acetate1 g300 · Experimental - Synthesis of polychelates
Partial recipeSource: Main

Route 2: Other

300 · Experimental - Synthesis of polychelates

Metal precursorscobalt(II) acetate tetrahydrate; 1.00 mmol
Linker precursorsH2BNESAP; 1.00 mmol
SolventsDMF, minimum quantity 25-30 ml for each solution
Additivessodium acetate, 1 g
Atmosphereair/not specified
Temperaturehot conditions; sand bath; dried at 80
Time3-4
Work-upFiltered; washed thoroughly with hot water, DMF, ethanol and acetone; dried in an oven at 80 C.
Activationdried in an oven at 80 C
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
Metal Sourcecobalt(II) acetate tetrahydrate1.00 mmol300 · Experimental - Synthesis of polychelates
LinkerH2BNESAP1.00 mmol300 · Experimental - Synthesis of polychelates
SolventDMF25-30 ml minimum quantity for each solution300 · Experimental - Synthesis of polychelates
Basesodium acetate1 g300 · Experimental - Synthesis of polychelates
Partial recipeSource: Main

Route 3: Other

300 · Experimental - Synthesis of polychelates

Metal precursorscopper(II) acetate monohydrate; 1.00 mmol
Linker precursorsH2BNESAP; 1.00 mmol
SolventsDMF, minimum quantity 25-30 ml for each solution
Additivessodium acetate, 1 g
Atmosphereair/not specified
Temperaturehot conditions; sand bath; dried at 80
Time3-4
Work-upFiltered; washed thoroughly with hot water, DMF, ethanol and acetone; dried in an oven at 80 C.
Activationdried in an oven at 80 C
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
Metal Sourcecopper(II) acetate monohydrate1.00 mmol300 · Experimental - Synthesis of polychelates
LinkerH2BNESAP1.00 mmol300 · Experimental - Synthesis of polychelates
SolventDMF25-30 ml minimum quantity for each solution300 · Experimental - Synthesis of polychelates
Basesodium acetate1 g300 · Experimental - Synthesis of polychelates
Partial recipeSource: Main

Route 4: Other

300 · Experimental - Synthesis of polychelates

Metal precursorsferrous ammonium sulfate; 1.00 mmol
Linker precursorsH2BNESAP; 1.00 mmol
SolventsDMF, minimum quantity 25-30 ml for each solution
Additivessodium acetate, 1 g
Atmosphereair/not specified
Temperaturehot conditions; sand bath; dried at 80
Time3-4
Work-upFiltered; washed thoroughly with hot water, DMF, ethanol and acetone; dried in an oven at 80 C.
Activationdried in an oven at 80 C
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
Metal Sourceferrous ammonium sulfate1.00 mmol300 · Experimental - Synthesis of polychelates
LinkerH2BNESAP1.00 mmol300 · Experimental - Synthesis of polychelates
SolventDMF25-30 ml minimum quantity for each solution300 · Experimental - Synthesis of polychelates
Basesodium acetate1 g300 · Experimental - Synthesis of polychelates
Partial recipeSource: Main

Route 5: Other

299 · Experimental - Synthesis of H2BNESAP

Linker precursorsIntermediate I; 1,2-diaminoethane
SolventsDMF; ethanol; 1:1 DMF-ethanol crystallisation mixture
Additivesdrop of concentrated H2SO4
Atmosphereair/not specified
Temperaturereflux on sand bath; numeric temperature not specified
Time3
Work-upCooled to room temperature; leaf-brown solid filtered, washed with DMF and ethanol, crystallised from 1:1 DMF-ethanol, dried in vacuo over calcium chloride.
Activationdried in vacuo over calcium chloride
Show 5 structured reagent records
RoleReagentAmount / concentrationSource
LinkerI0.05 mol299 · Experimental - Synthesis of H2BNESAP
SolventDMF25 ml299 · Experimental - Synthesis of H2BNESAP
Linker1,2-diaminoethane0.05 mol299 · Experimental - Synthesis of H2BNESAP
Solventethanol25 ml299 · Experimental - Synthesis of H2BNESAP
Acidconcentrated H2SO4a drop299 · Experimental - Synthesis of H2BNESAP
Partial recipeSource: Main

Route 6: Other

299 · Experimental - Synthesis of I

Linker precursorsbenzidine; salicylaldehyde
Solventswater
Additivesconc. HCl; sodium nitrite; sodium carbonate
Atmosphereair/not specified
Temperaturebelow 10
Time3-4 h plus additional coupling/stirring time
Oxidant / reductantsodium nitrite
Work-upAcidified with cold dilute hydrochloric acid; precipitate filtered, washed and dried under vacuum at 60 C; purity checked by TLC.
Activationdried under vacuum at 60 C
Show 6 structured reagent records
RoleReagentAmount / concentrationSource
Linkerfinely powdered benzidine9.52 g, 0.05 mol299 · Experimental - Synthesis of I
Solventwater150 ml + 15 ml + 50 ml + 20 ml299 · Experimental - Synthesis of I
Acidconc. HCl5 ml then further 5 ml299 · Experimental - Synthesis of I
Oxidantsodium nitrite3.5 g, 0.05 mol299 · Experimental - Synthesis of I
Linkersalicylaldehyde0.05 mol then second 0.05 mol299 · Experimental - Synthesis of I
Basesodium carbonate15 g then 3 g299 · Experimental - Synthesis of I
Partial recipeSource: Main

Route 7: Other

300 · Experimental - Synthesis of polychelates

Metal precursorsManganese(II) acetate tetrahydrate; 1.00 mmol
Linker precursorsH2BNESAP; 1.00 mmol
SolventsDMF, minimum quantity 25-30 ml for each solution
Additivessodium acetate, 1 g
Atmosphereair/not specified
Temperaturehot conditions; sand bath; dried at 80
Time3-4
Work-upFiltered; washed thoroughly with hot water, DMF, ethanol and acetone; dried in an oven at 80 C.
Activationdried in an oven at 80 C
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceManganese(II) acetate tetrahydrate1.00 mmol300 · Experimental - Synthesis of polychelates
LinkerH2BNESAP1.00 mmol300 · Experimental - Synthesis of polychelates
SolventDMF25-30 ml minimum quantity for each solution300 · Experimental - Synthesis of polychelates
Basesodium acetate1 g300 · Experimental - Synthesis of polychelates
Partial recipeSource: Main

Route 8: Other

300 · Experimental - Synthesis of polychelates

Metal precursorsnickel(II) acetate tetrahydrate; 1.00 mmol
Linker precursorsH2BNESAP; 1.00 mmol
SolventsDMF, minimum quantity 25-30 ml for each solution
Additivessodium acetate, 1 g
Atmosphereair/not specified
Temperaturehot conditions; sand bath; dried at 80
Time3-4
Work-upFiltered; washed thoroughly with hot water, DMF, ethanol and acetone; dried in an oven at 80 C.
Activationdried in an oven at 80 C
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
Metal Sourcenickel(II) acetate tetrahydrate1.00 mmol300 · Experimental - Synthesis of polychelates
LinkerH2BNESAP1.00 mmol300 · Experimental - Synthesis of polychelates
SolventDMF25-30 ml minimum quantity for each solution300 · Experimental - Synthesis of polychelates
Basesodium acetate1 g300 · Experimental - Synthesis of polychelates
Partial recipeSource: Main

Route 9: Other

300 · Experimental - Synthesis of polychelates

Metal precursorszinc(II) acetate dihydrate; 1.00 mmol
Linker precursorsH2BNESAP; 1.00 mmol
SolventsDMF, minimum quantity 25-30 ml for each solution
Additivessodium acetate, 1 g
Atmosphereair/not specified
Temperaturehot conditions; sand bath; dried at 80
Time3-4
Work-upFiltered; washed thoroughly with hot water, DMF, ethanol and acetone; dried in an oven at 80 C.
Activationdried in an oven at 80 C
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
Metal Sourcezinc(II) acetate dihydrate1.00 mmol300 · Experimental - Synthesis of polychelates
LinkerH2BNESAP1.00 mmol300 · Experimental - Synthesis of polychelates
SolventDMF25-30 ml minimum quantity for each solution300 · Experimental - Synthesis of polychelates
Basesodium acetate1 g300 · Experimental - Synthesis of polychelates