Synthesis evidence

New coordination polymers of 1,4-bis(2′-hydroxyphenylazomethine) phenylene

Hassan M.K., Abd-Alla M.A., Hasan R.M. · Journal of Macromolecular Science: Part A - Chemistry · 1990 · 1501-1512

7 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

1502 · Experimental · Synthesis of BHPAP

Metal precursorsnone
Linker precursorso-aminophenol; terephthaldehyde
Solvents100 mL absolute ethanol; ethanol for washing and recrystallisation
Additivesnone reported
Atmospherenot reported
Temperature60
Time0.5
Work-upProduct filtered off, washed with ethanol, dried, and recrystallised from ethanol.
Activationdrying reported; no activation step reported
Scalability context95% yield reported.
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
Othero-aminophenol0.2 mol1502 · Experimental · Synthesis of BHPAP
Linkerterephthaldehyde0.1 mol1502 · Experimental · Synthesis of BHPAP
Solventabsolute ethanol100 mL1502 · Experimental · Synthesis of BHPAP
Partial recipeSource: Main

Route 2: Other

1503-1504 · Experimental; Results and Discussion · Preparation of Polychelates

Metal precursorsCr(III) chloride (exact salt/hydrate not specified)
Linker precursorsBHPAP ligand
Solventsethanol; ethyl alcohol wash
Additivesfew drops of DMF as HCl scavenger
Atmospherenot reported; products stable in air
Temperature70
Time2
Work-upProduct separated, filtered off, washed thoroughly with ethyl alcohol, then dried under vacuum over phosphorus pentoxide.
Activationdried under vacuum over phosphorus pentoxide
Scalability contextQuantitative yields reported for the desired polymeric chelates.
Show 6 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceCr(III) chloride0.01 mol1503-1504 · Experimental; Results and Discussion · Preparation of Polychelates
LinkerBHPAP0.01 mol1503-1504 · Experimental; Results and Discussion · Preparation of Polychelates
Solventethanolnot reported1503-1504 · Experimental; Results and Discussion · Preparation of Polychelates
AdditiveDMFa few drops1503-1504 · Experimental; Results and Discussion · Preparation of Polychelates
Solventethyl alcoholwash solvent1503-1504 · Experimental; Results and Discussion · Preparation of Polychelates
Otherphosphorus pentoxidedrying agent1503-1504 · Experimental; Results and Discussion · Preparation of Polychelates
Partial recipeSource: Main

Route 3: Other

1503-1504 · Experimental; Results and Discussion · Preparation of Polychelates

Metal precursorsCu(II) chloride (exact salt/hydrate not specified)
Linker precursorsBHPAP ligand
Solventsethanol; ethyl alcohol wash
Additivesfew drops of DMF as HCl scavenger
Atmospherenot reported; products stable in air
Temperature70
Time2
Work-upProduct separated, filtered off, washed thoroughly with ethyl alcohol, then dried under vacuum over phosphorus pentoxide.
Activationdried under vacuum over phosphorus pentoxide
Scalability contextQuantitative yields reported for the desired polymeric chelates.
Show 6 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceCu(II) chloride0.01 mol1503-1504 · Experimental; Results and Discussion · Preparation of Polychelates
LinkerBHPAP0.01 mol1503-1504 · Experimental; Results and Discussion · Preparation of Polychelates
Solventethanolnot reported1503-1504 · Experimental; Results and Discussion · Preparation of Polychelates
AdditiveDMFa few drops1503-1504 · Experimental; Results and Discussion · Preparation of Polychelates
Solventethyl alcoholwash solvent1503-1504 · Experimental; Results and Discussion · Preparation of Polychelates
Otherphosphorus pentoxidedrying agent1503-1504 · Experimental; Results and Discussion · Preparation of Polychelates
Partial recipeSource: Main

Route 4: Other

1503-1504 · Experimental; Results and Discussion · Preparation of Polychelates

Metal precursorsFe(III) chloride (exact salt/hydrate not specified)
Linker precursorsBHPAP ligand
Solventsethanol; ethyl alcohol wash
Additivesfew drops of DMF as HCl scavenger
Atmospherenot reported; products stable in air
Temperature70
Time2
Work-upProduct separated, filtered off, washed thoroughly with ethyl alcohol, then dried under vacuum over phosphorus pentoxide.
Activationdried under vacuum over phosphorus pentoxide
Scalability contextQuantitative yields reported for the desired polymeric chelates.
Show 6 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceFe(III) chloride0.01 mol1503-1504 · Experimental; Results and Discussion · Preparation of Polychelates
LinkerBHPAP0.01 mol1503-1504 · Experimental; Results and Discussion · Preparation of Polychelates
Solventethanolnot reported1503-1504 · Experimental; Results and Discussion · Preparation of Polychelates
AdditiveDMFa few drops1503-1504 · Experimental; Results and Discussion · Preparation of Polychelates
Solventethyl alcoholwash solvent1503-1504 · Experimental; Results and Discussion · Preparation of Polychelates
Otherphosphorus pentoxidedrying agent1503-1504 · Experimental; Results and Discussion · Preparation of Polychelates
Partial recipeSource: Main

Route 5: Other

1503-1504 · Experimental; Results and Discussion · Preparation of Polychelates

Metal precursorsMn(II) chloride (exact salt/hydrate not specified)
Linker precursorsBHPAP ligand
Solventsethanol; ethyl alcohol wash
Additivesfew drops of DMF as HCl scavenger
Atmospherenot reported; products stable in air
Temperature70
Time2
Work-upProduct separated, filtered off, washed thoroughly with ethyl alcohol, then dried under vacuum over phosphorus pentoxide.
Activationdried under vacuum over phosphorus pentoxide
Scalability contextQuantitative yields reported for the desired polymeric chelates.
Show 6 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceMn(II) chloride0.01 mol1503-1504 · Experimental; Results and Discussion · Preparation of Polychelates
LinkerBHPAP0.01 mol1503-1504 · Experimental; Results and Discussion · Preparation of Polychelates
Solventethanolnot reported1503-1504 · Experimental; Results and Discussion · Preparation of Polychelates
AdditiveDMFa few drops1503-1504 · Experimental; Results and Discussion · Preparation of Polychelates
Solventethyl alcoholwash solvent1503-1504 · Experimental; Results and Discussion · Preparation of Polychelates
Otherphosphorus pentoxidedrying agent1503-1504 · Experimental; Results and Discussion · Preparation of Polychelates
Partial recipeSource: Main

Route 6: Other

1503-1504 · Experimental; Results and Discussion · Preparation of Polychelates

Metal precursorsNi(II) chloride (exact salt/hydrate not specified)
Linker precursorsBHPAP ligand
Solventsethanol; ethyl alcohol wash
Additivesfew drops of DMF as HCl scavenger
Atmospherenot reported; products stable in air
Temperature70
Time2
Work-upProduct separated, filtered off, washed thoroughly with ethyl alcohol, then dried under vacuum over phosphorus pentoxide.
Activationdried under vacuum over phosphorus pentoxide
Scalability contextQuantitative yields reported for the desired polymeric chelates.
Show 6 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceNi(II) chloride0.01 mol1503-1504 · Experimental; Results and Discussion · Preparation of Polychelates
LinkerBHPAP0.01 mol1503-1504 · Experimental; Results and Discussion · Preparation of Polychelates
Solventethanolnot reported1503-1504 · Experimental; Results and Discussion · Preparation of Polychelates
AdditiveDMFa few drops1503-1504 · Experimental; Results and Discussion · Preparation of Polychelates
Solventethyl alcoholwash solvent1503-1504 · Experimental; Results and Discussion · Preparation of Polychelates
Otherphosphorus pentoxidedrying agent1503-1504 · Experimental; Results and Discussion · Preparation of Polychelates
Partial recipeSource: Main

Route 7: Other

1503-1504 · Experimental; Results and Discussion · Preparation of Polychelates

Metal precursorsTi(III) chloride (exact salt/hydrate not specified)
Linker precursorsBHPAP ligand
Solventsethanol; ethyl alcohol wash
Additivesfew drops of DMF as HCl scavenger
Atmospherenot reported; products stable in air
Temperature70
Time2
Work-upProduct separated, filtered off, washed thoroughly with ethyl alcohol, then dried under vacuum over phosphorus pentoxide.
Activationdried under vacuum over phosphorus pentoxide
Scalability contextQuantitative yields reported for the desired polymeric chelates.
Show 6 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceTi(III) chloride0.01 mol1503-1504 · Experimental; Results and Discussion · Preparation of Polychelates
LinkerBHPAP0.01 mol1503-1504 · Experimental; Results and Discussion · Preparation of Polychelates
Solventethanolnot reported1503-1504 · Experimental; Results and Discussion · Preparation of Polychelates
AdditiveDMFa few drops1503-1504 · Experimental; Results and Discussion · Preparation of Polychelates
Solventethyl alcoholwash solvent1503-1504 · Experimental; Results and Discussion · Preparation of Polychelates
Otherphosphorus pentoxidedrying agent1503-1504 · Experimental; Results and Discussion · Preparation of Polychelates