cMOF Evidence Base

Synthesis evidence

In Situ Oxidation of Pyridyl-Dihydrobenzoimidazoquinazoline and the Synthesis of a Highly Luminescent Cd(II) Coordination Polymer: A Promising Candidate for Mutagenic Nitroaromatic Detection and Device Fabrication

Bairy G., Das P., Dutta B. et al. · Inorganic Chemistry · 2023 · 12773-12782

4 structured synthesis routes

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

Partial recipeSource: SI

Route 1: Other

p020 / SI page 20 · Device Fabrication

Solventsacetone; ethanol; distilled water; DMF
AtmosphereN2 drying atmosphere; vacuum deposition at 10-6 Torr
Temperatureroom temperature
Substrate orientationITO-coated glass substrate
Work-upITO glass ultrasonically cleaned with acetone, ethanol and distilled water; dried under N2; compound 1 dispersed/dissolved in DMF and ultrasonicated; spin-coated on ITO; Al deposited by electron-beam vacuum coating using a shadow mask.
Scalability contextEffective diode area 7.065 x 10-6 m2; film thickness 1 micrometre. Spin speed/time and precursor concentration are not reported.
Show 7 structured reagent records
RoleReagentAmount / concentrationSource
Othercompound 1Not specifiedp020 / SI page 20 · Device Fabrication
SolventDMFNot specifiedp020 / SI page 20 · Device Fabrication
Solventacetonesubstrate cleaningp020 / SI page 20 · Device Fabrication
Solventethanolsubstrate cleaningp020 / SI page 20 · Device Fabrication
Solventdistilled watersubstrate cleaningp020 / SI page 20 · Device Fabrication
OtherITO-coated glass substrateNot specifiedp020 / SI page 20 · Device Fabrication
Otheraluminiumtop contact deposited by electron beamp020 / SI page 20 · Device Fabrication
Complete recipeSource: Both

Route 2: Liquid Liquid Interface

p003 / journal page 12775 · Synthesis of [Cd(glu)2(pbiq)2(H2O)]n (1) · Scheme S2

Metal precursorsCd(NO3)2.4H2O
Linker precursorsH2pbiq; glutaric acid (H2glu)
SolventsH2O; MeOH; EtOH; H2O/MeOH (1:1 v/v) buffer layer
AdditivesEt3N
Atmosphereambient air; in situ aerial oxidation reported
Temperatureroom temperature
Time240
Oxidant / reductantO2 from air inferred as oxidant for in situ aerial oxidation of H2pbiq to pbiq
Work-upLayered solution left to dissipate; after 10 days block-like yellow crystals collected.
Scalability contextCd(II) compounds were handled carefully and prepared in small quantities.
Show 7 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceCd(NO3)2.4H2O61.7 mg, 0.2 mmolp003 / journal page 12775 · Synthesis of [Cd(glu)2(pbiq)2(H2O)]n (1) · Scheme S2
LinkerH2pbiq59.6 mg, 0.2 mmol in aqueous solutionp003 / journal page 12775 · Synthesis of [Cd(glu)2(pbiq)2(H2O)]n (1) · Scheme S2
Linkerglutaric acid26.4 mg, 0.2 mmol in EtOH (2 mL)p003 / journal page 12775 · Synthesis of [Cd(glu)2(pbiq)2(H2O)]n (1) · Scheme S2
BaseEt3N21 mg, 0.2 mmolp003 / journal page 12775 · Synthesis of [Cd(glu)2(pbiq)2(H2O)]n (1) · Scheme S2
SolventH2O/MeOH1:1 v/v buffer solutionp003 / journal page 12775 · Synthesis of [Cd(glu)2(pbiq)2(H2O)]n (1) · Scheme S2
SolventH2O2 mL for H2pbiq solutionp003 / journal page 12775 · Synthesis of [Cd(glu)2(pbiq)2(H2O)]n (1) · Scheme S2
SolventEtOH2 mL for glutaric acid solutionp003 / journal page 12775 · Synthesis of [Cd(glu)2(pbiq)2(H2O)]n (1) · Scheme S2
Complete recipeSource: Both

Route 3: Other

p003 / journal page 12775 · Synthesis of Ligand (H2pbiq) · Scheme S1

Linker precursors2-(1H-benzo[d]imidazol-2-yl)aniline; pyridine-4-carbaldehyde
Solventsethanol; ethyl acetate/hexane (3:7 v/v) for chromatography
Additivesanhydrous Na2SO4 for drying
Temperaturereflux
Time6
Work-upCooled to room temperature; concentrated at low pressure; dried over anhydrous Na2SO4; concentrated under reduced pressure; purified by column chromatography.
Show 5 structured reagent records
RoleReagentAmount / concentrationSource
Linker2-(1H-benzo[d]imidazol-2-yl)aniline209 mg, 1.0 mmolp003 / journal page 12775 · Synthesis of Ligand (H2pbiq) · Scheme S1
Linkerpyridine-4-carbaldehyde107 mg, 1.0 mmolp003 / journal page 12775 · Synthesis of Ligand (H2pbiq) · Scheme S1
Solventethanol5 mLp003 / journal page 12775 · Synthesis of Ligand (H2pbiq) · Scheme S1
Solventethyl acetate/hexane3:7 v/v, chromatography eluentp003 / journal page 12775 · Synthesis of Ligand (H2pbiq) · Scheme S1
Additiveanhydrous Na2SO4Not specifiedp003 / journal page 12775 · Synthesis of Ligand (H2pbiq) · Scheme S1
Complete recipeSource: SI

Route 4: Other

p005 / SI page 5 · Synthesis of pbiq · Scheme S3

Linker precursorsH2pbiq
SolventsDMF; water; ethyl acetate/hexane (2:3 v/v) for chromatography
Atmosphereair bubbled through reaction mixture
Temperaturereflux
Time2
Oxidant / reductantair/O2 as oxidant
Work-upPoured into water (30 mL); light yellow precipitate filtered; crude product purified by column chromatography with ethyl acetate/hexane (2:3 v/v).
Show 5 structured reagent records
RoleReagentAmount / concentrationSource
LinkerH2pbiq89.4 mg, 0.3 mmolp005 / SI page 5 · Synthesis of pbiq · Scheme S3
SolventDMF3 mLp005 / SI page 5 · Synthesis of pbiq · Scheme S3
Oxidantairbubbled through reaction mixturep005 / SI page 5 · Synthesis of pbiq · Scheme S3
Solventwater30 mL workupp005 / SI page 5 · Synthesis of pbiq · Scheme S3
Solventethyl acetate/hexane2:3 v/v, chromatography eluentp005 / SI page 5 · Synthesis of pbiq · Scheme S3