Synthesis evidence

4′-((4-cyanobenzyl)oxy)-[1,1′-biphenyl] -4-carboxylic acid based Cd(II), Co(II), Mn(II) and Ni(II) coordination polymers as photocatalyst for nitrofurazone degradation

Wang X., Kumar Ghosh M., Zhuang P. et al. · Inorganica Chimica Acta · 2024 · 121892

4 structured synthesis routes

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

Complete recipeSource: Both

Route 1: Hydrothermal

4 · 2.2.1 Synthesis of 1

Metal precursorsCd(NO3)2.4H2O (0.0308 g, 0.1 mmol)
Linker precursorsHL (0.0329 g, 0.1 mmol); 4,4'-bis(imidazolyl)biphenyl (bbp) (0.0286 g, 0.1 mmol)
Solvents4 mL CH3CN and 4 mL double-distilled water
AtmosphereAir during 30 min agitation; sealed Teflon-lined vessel during heating
Temperature140
Time72
Work-upCooled at 5 deg C/h to give yellow block crystals; isolated product yield 41% based on Cd.
ActivationNot reported
Scalability contextSmall sealed-vessel crystal synthesis; no scale-up data reported.
Show 5 structured reagent records
RoleReagentAmount / concentrationSource
Linker4'-((4-cyanobenzyl)oxy)-[1,1'-biphenyl]-4-carboxylic acid (HL)0.0329 g, 0.1 mmol4 · 2.2.1 Synthesis of 1
Linker4,4'-bis(imidazolyl)biphenyl (bbp)0.0286 g, 0.1 mmol4 · 2.2.1 Synthesis of 1
Metal SourceCd(NO3)2.4H2O0.0308 g, 0.1 mmol4 · 2.2.1 Synthesis of 1
SolventCH3CN4 mL4 · 2.2.1 Synthesis of 1
Solventdouble distilled water4 mL4 · 2.2.1 Synthesis of 1
Complete recipeSource: Both

Route 2: Hydrothermal

4 · 2.2.2 Synthesis of 2

Metal precursorsCo(NO3).6H2O (0.0291 g, 0.1 mmol)
Linker precursorsHL (0.0329 g, 0.1 mmol); bbp (0.0286 g, 0.1 mmol)
Solvents4 mL CH3CN and 4 mL double-distilled water
AtmosphereAir during 30 min agitation; sealed Teflon-lined vessel during heating
Temperature140
Time72
Work-upCooled at 5 deg C/h to give purple block crystals; isolated product yield 55% as reported.
ActivationNot reported
Scalability contextSmall sealed-vessel crystal synthesis; no scale-up data reported.
Show 5 structured reagent records
RoleReagentAmount / concentrationSource
Linker4'-((4-cyanobenzyl)oxy)-[1,1'-biphenyl]-4-carboxylic acid (HL)0.0329 g, 0.1 mmol4 · 2.2.2 Synthesis of 2
Linker4,4'-bis(imidazolyl)biphenyl (bbp)0.0286 g, 0.1 mmol4 · 2.2.2 Synthesis of 2
Metal SourceCo(NO3).6H2O0.0291 g, 0.1 mmol4 · 2.2.2 Synthesis of 2
SolventCH3CN4 mL4 · 2.2.2 Synthesis of 2
Solventdouble distilled water4 mL4 · 2.2.2 Synthesis of 2
Complete recipeSource: Both

Route 3: Hydrothermal

4 · 2.2.3 Synthesis of 3

Metal precursorsMn(ClO4)2.6H2O (0.0362 g, 0.1 mmol)
Linker precursorsHL (0.0329 g, 0.1 mmol); bbp (0.0286 g, 0.1 mmol)
Solvents4 mL CH3CN and 4 mL double-distilled water
AtmosphereAir during 30 min agitation; sealed Teflon-lined vessel during heating
Temperature140
Time72
Work-upCooled at 5 deg C/h to give pink block crystals; isolated product yield 48% based on Mn.
ActivationNot reported
Scalability contextSmall sealed-vessel crystal synthesis; no scale-up data reported.
Show 5 structured reagent records
RoleReagentAmount / concentrationSource
Linker4'-((4-cyanobenzyl)oxy)-[1,1'-biphenyl]-4-carboxylic acid (HL)0.0329 g, 0.1 mmol4 · 2.2.3 Synthesis of 3
Linker4,4'-bis(imidazolyl)biphenyl (bbp)0.0286 g, 0.1 mmol4 · 2.2.3 Synthesis of 3
Metal SourceMn(ClO4)2.6H2O0.0362 g, 0.1 mmol4 · 2.2.3 Synthesis of 3
SolventCH3CN4 mL4 · 2.2.3 Synthesis of 3
Solventdouble distilled water4 mL4 · 2.2.3 Synthesis of 3
Complete recipeSource: Both

Route 4: Hydrothermal

4 · 2.2.4 Synthesis of 4

Metal precursorsNi(NO3)2.6H2O (0.0291 g, 0.1 mmol)
Linker precursorsHL (0.0329 g, 0.1 mmol); bbp (0.0286 g, 0.1 mmol)
Solvents4 mL CH3CN and 4 mL double-distilled water
AtmosphereAir during 30 min agitation; sealed Teflon-lined vessel during heating
Temperature140
Time72
Work-upCooled at 5 deg C/h to give green block crystals; isolated product yield 60% based on Ni.
ActivationNot reported
Scalability contextSmall sealed-vessel crystal synthesis; no scale-up data reported.
Show 5 structured reagent records
RoleReagentAmount / concentrationSource
Linker4'-((4-cyanobenzyl)oxy)-[1,1'-biphenyl]-4-carboxylic acid (HL)0.0329 g, 0.1 mmol4 · 2.2.4 Synthesis of 4
Linker4,4'-bis(imidazolyl)biphenyl (bbp)0.0286 g, 0.1 mmol4 · 2.2.4 Synthesis of 4
Metal SourceNi(NO3)2.6H2O0.0291 g, 0.1 mmol4 · 2.2.4 Synthesis of 4
SolventCH3CN4 mL4 · 2.2.4 Synthesis of 4
Solventdouble distilled water4 mL4 · 2.2.4 Synthesis of 4