cMOF Evidence Base

Synthesis evidence

An examination of some active organometallic substances for ion-selective electrodes

Sharp M. · Analytica Chimica Acta · 1975 · 165-176

10 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

p005 / journal page 169 · Experimental; Coordination polymers

Metal precursorscadmium acetate plus iron(III) source not specified
Linker precursorschloranil; o-phenylenediamine
Solventshot ethanol and water used for washing
Atmospheredry nitrogen
Temperature250
Time0.5
Work-upProduct washed after synthesis; Fe(III) addition increased cross-linking and stability.
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
Metal Sourcecadmium acetateNot specifiedp005 / journal page 169 · Experimental; Coordination polymers
Metal Sourceiron(III) sourcenot specifiedp005 / journal page 169 · Experimental; Coordination polymers
Linkerchloranil and o-phenylenediamine1:2 molar ratio in general routep005 / journal page 169 · Experimental; Coordination polymers
Partial recipeSource: Main

Route 2: Other

p004-p005 / journal pages 168-169 · Experimental; Coordination polymers · Fig. 4

Metal precursorsmetal acetate (Cu, Cd, or Cd plus Fe(III))
Linker precursorschloranil; o-phenylenediamine
Solventshot ethanol and water used for washing
Atmospheredry nitrogen
Temperature250
Time0.5
Work-upResulting product was crushed and washed with large quantities of hot ethanol and water.
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
Linkerchloranil1 molep004-p005 / journal pages 168-169 · Experimental; Coordination polymers · Fig. 4
Linkero-phenylenediamine2 molesp004-p005 / journal pages 168-169 · Experimental; Coordination polymers · Fig. 4
Metal Sourcemetal acetate1 molep004-p005 / journal pages 168-169 · Experimental; Coordination polymers · Fig. 4
Solventhot ethanol and waterlarge quantitiesp004-p005 / journal pages 168-169 · Experimental; Coordination polymers · Fig. 4
Partial recipeSource: Main

Route 3: Other

p004 / journal page 168 · Experimental; Metal-phthalocyanines

Metal precursorsLi2Pc precursor; copper salt not specified
Linker precursorsphthalocyanine ligand generated from phthalonitrile
Solventsethanol for double decomposition
Work-upCuPc precipitated from ethanol solution.
Show 2 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceLi2PcNot specifiedp004 / journal page 168 · Experimental; Metal-phthalocyanines
SolventethanolNot specifiedp004 / journal page 168 · Experimental; Metal-phthalocyanines
Vague recipeSource: Main

Route 4: Other

p004 / journal page 168 · Experimental; Tetracyanoethylene (TCNE) polymers

Metal precursorscopper, nickel, or zinc metal source not specified; prepared similarly to Mg-TCNE
Linker precursorstetracyanoethylene (TCNE)
Solventsnitrobenzene; concentrated sulphuric acid; ice-water
Temperaturereflux in nitrobenzene; dried at 60-70 C by analogy to Mg-TCNE
Timeapproximately 10 h by analogy to Mg-TCNE
Work-upPrepared similarly to Mg-TCNE; details inherited only by analogy.
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
LinkerTCNEnot separately specifiedp004 / journal page 168 · Experimental; Tetracyanoethylene (TCNE) polymers
Metal Sourcecopper, nickel or zinc sourcenot separately specifiedp004 / journal page 168 · Experimental; Tetracyanoethylene (TCNE) polymers
Solventnitrobenzenenot separately specifiedp004 / journal page 168 · Experimental; Tetracyanoethylene (TCNE) polymers
Partial recipeSource: Main

Route 5: Other

p004 / journal page 168 · Experimental; Tetracyanoethylene (TCNE) polymers

Metal precursorsfinely divided magnesium
Linker precursorstetracyanoethylene (TCNE)
Solventsnitrobenzene; concentrated sulphuric acid; ice-water
Temperaturereflux in nitrobenzene; dried at 60-70 C
Timeapproximately 10 h reflux
Work-upBlack infusible product filtered or dissolved in concentrated sulphuric acid, reprecipitated into ice-water, filtered again, and oven-dried at 60-70 C.
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
LinkerTCNE (Eastman Kodak Co.)3 gp004 / journal page 168 · Experimental; Tetracyanoethylene (TCNE) polymers
Metal Sourcefinely divided magnesium0.57 gp004 / journal page 168 · Experimental; Tetracyanoethylene (TCNE) polymers
Solventnitrobenzene20 mlp004 / journal page 168 · Experimental; Tetracyanoethylene (TCNE) polymers
Acidconcentrated sulphuric acidNot specifiedp004 / journal page 168 · Experimental; Tetracyanoethylene (TCNE) polymers
Vague recipeSource: Main

Route 6: Other

p004 / journal page 168 · Experimental; Tetracyanoethylene (TCNE) polymers

Metal precursorsnickel metal source not specified; prepared similarly to Mg-TCNE
Linker precursorstetracyanoethylene (TCNE)
Solventsnitrobenzene; concentrated sulphuric acid; ice-water
Temperaturereflux in nitrobenzene; dried at 60-70 C by analogy to Mg-TCNE
Timeapproximately 10 h by analogy to Mg-TCNE
Work-upPrepared similarly to Mg-TCNE; details inherited only by analogy.
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
LinkerTCNEnot separately specifiedp004 / journal page 168 · Experimental; Tetracyanoethylene (TCNE) polymers
Metal Sourcenickel sourcenot separately specifiedp004 / journal page 168 · Experimental; Tetracyanoethylene (TCNE) polymers
Solventnitrobenzenenot separately specifiedp004 / journal page 168 · Experimental; Tetracyanoethylene (TCNE) polymers
Partial recipeSource: Main

Route 7: Other

p004 / journal page 168 · Experimental; Metal-phthalocyanines

Metal precursorsLi2Pc precursor; lead salt not specified
Linker precursorsphthalocyanine ligand generated from phthalonitrile
Solventsamyl alcohol for Li2Pc preparation; ethanol for double decomposition
Work-upLi2Pc isolated as a blue solid; PbPc and CuPc products precipitated from ethanol solution.
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
Linkerphthalonitrile30 gp004 / journal page 168 · Experimental; Metal-phthalocyanines
Metal Sourcelithium2 gp004 / journal page 168 · Experimental; Metal-phthalocyanines
Solventamyl alcohol150 mlp004 / journal page 168 · Experimental; Metal-phthalocyanines
SolventethanolNot specifiedp004 / journal page 168 · Experimental; Metal-phthalocyanines
Partial recipeSource: Main

Route 8: Other

p005 / journal page 169 · Experimental; Electrodes

Metal precursorscommercial Ph3PbBr converted to Ph3PbOH
Linker precursorsphenyl groups already present in Ph3PbBr
Solventsethanol or ethanol-water mixtures for metathesis; o-dichlorobenzene for membrane solution
Additivescarbonate sodium salt; sodium hydroxide
Work-upWhite water-insoluble solid dissolved in o-dichlorobenzene to form a liquid membrane.
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourcePh3PbBrNot specifiedp005 / journal page 169 · Experimental; Electrodes
Basesodium hydroxideNot specifiedp005 / journal page 169 · Experimental; Electrodes
Additivecarbonate sodium saltNot specifiedp005 / journal page 169 · Experimental; Electrodes
Solvento-dichlorobenzene1.86 g l-1 (Ph3Pb)2CO3 membrane solutionp005 / journal page 169 · Experimental; Electrodes
Partial recipeSource: Main

Route 9: Other

p003 / journal page 167 · Experimental; Organolead salts

Metal precursorscommercial Ph3PbBr
Linker precursorsphenyl groups already present in Ph3PbBr
Solventsethanol or ethanol-water mixtures for metathesis; o-dichlorobenzene for membrane solution
Additivesappropriate sodium salts; sodium hydroxide
Work-upMetathesis afforded white water-insoluble solids; dissolved in o-dichlorobenzene for liquid membranes.
Show 5 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourcePh3PbBrNot specifiedp003 / journal page 167 · Experimental; Organolead salts
Basesodium hydroxideNot specifiedp003 / journal page 167 · Experimental; Organolead salts
Additiveappropriate sodium saltsNot specifiedp003 / journal page 167 · Experimental; Organolead salts
Solventethanol or ethanol-water mixturesNot specifiedp003 / journal page 167 · Experimental; Organolead salts
Solvento-dichlorobenzene9.77 g l-1 (Ph3Pb)2SO4 membrane solutionp003 / journal page 167 · Experimental; Organolead salts
Vague recipeSource: Main

Route 10: Other

p004 / journal page 168 · Experimental; Tetracyanoethylene (TCNE) polymers

Metal precursorszinc metal source not specified; prepared similarly to Mg-TCNE
Linker precursorstetracyanoethylene (TCNE)
Solventsnitrobenzene; concentrated sulphuric acid; ice-water
Temperaturereflux in nitrobenzene; dried at 60-70 C by analogy to Mg-TCNE
Timeapproximately 10 h by analogy to Mg-TCNE
Work-upPrepared similarly to Mg-TCNE; details inherited only by analogy.
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
LinkerTCNEnot separately specifiedp004 / journal page 168 · Experimental; Tetracyanoethylene (TCNE) polymers
Metal Sourcezinc sourcenot separately specifiedp004 / journal page 168 · Experimental; Tetracyanoethylene (TCNE) polymers
Solventnitrobenzenenot separately specifiedp004 / journal page 168 · Experimental; Tetracyanoethylene (TCNE) polymers