Synthesis evidence

2D Cd(II)-MOF of Pyridyl-Imidazoquinazoline: Structure, Luminescence, and Selective Detection of TNP and Fabrication of Semiconducting Devices

Bairy G., Dey A., Dutta B. et al. · Crystal Growth and Design · 2022 · 3138-3147

3 structured synthesis routes

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

Partial recipeSource: Both

Route 1: Liquid Liquid Interface

p003 / article p.3140 · Experimental Section - Synthesis of CP 1 · Scheme S2

Metal precursorsCd(NO3)2·4H2O
Linker precursorspdiq; 5-nitroisophthalic acid (H2nip)
SolventsMeOH, H2O, EtOH; MeOH/H2O 1:1 buffer layer
AdditivesEt3N neutralising base
Atmosphereambient air; not otherwise specified
Temperatureambient temperature; exact value not specified
Timeabout 120 h (five days)
Work-upCrystals isolated after diffusion; no washing, drying, or activation procedure reported for CP 1 crystals.
Activationnone reported
Scalability context0.2 mmol metal/linker scale; 164 mg product, 62% yield.
Show 7 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceCd(NO3)2·4H2O61.7 mg, 0.2 mmolp003 / article p.3140 · Experimental Section - Synthesis of CP 1 · Scheme S2
Linkerpdiq59.6 mg, 0.2 mmolp003 / article p.3140 · Experimental Section - Synthesis of CP 1 · Scheme S2
Linker5-nitroisophthalic acid42 mg, 0.2 mmolp003 / article p.3140 · Experimental Section - Synthesis of CP 1 · Scheme S2
BaseEt3N21 mg, 0.2 mmolp003 / article p.3140 · Experimental Section - Synthesis of CP 1 · Scheme S2
SolventMeOH2 mL for pdiq plus 1:1 MeOH/H2O buffer layerp003 / article p.3140 · Experimental Section - Synthesis of CP 1 · Scheme S2
SolventH2O2 mL for Cd solution plus 1:1 MeOH/H2O buffer layerp003 / article p.3140 · Experimental Section - Synthesis of CP 1 · Scheme S2
SolventEtOH2 mL for 5-nitroisophthalic acid solutionp003 / article p.3140 · Experimental Section - Synthesis of CP 1 · Scheme S2
Partial recipeSource: SI

Route 2: Other

p015 · Device Fabrication

Metal precursorsas-synthesised CP 1
Linker precursorsnot applicable; uses preformed CP 1
Solventsnot specified for doctor-blade coating
AdditivesAl metal electrode
Atmosphereambient for fabrication/measurements; Al deposition under 10^-6 Torr
Temperatureroom temperature
Timenot specified
Substrate orientationpre-cleaned ITO-coated glass substrate
Work-upDoctor-blade growth of CP 1 thin film on ITO-coated glass; aluminium deposited on plain glass slide in vacuum coating unit under 10^-6 Torr as metal electrode.
Activationnone reported
Scalability contextMultiple MS junction devices were developed; no device area or coating concentration reported.
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
Otheras-synthesized CP 1not specifiedp015 · Device Fabrication
OtherITO coated glass substratenot specifiedp015 · Device Fabrication
Otheraluminium electrodenot specified · deposited under 10^-6 Torrp015 · Device Fabrication
Complete recipeSource: Both

Route 3: Other

p003 / article p.3140 · Experimental Section - Synthesis of the Ligand (pdiq) · Scheme S1

Linker precursors2-(1H-benzo[d]imidazol-2-yl) aniline; isonicotinaldehyde
Solventsethanol; ethyl acetate; hexane
Additivesanhydrous Na2SO4 drying agent
Atmospherenot specified
Temperaturereflux; exact temperature not reported
Time6
Work-upCooled to ambient temperature, concentrated under reduced pressure, diluted with ethyl acetate, dried over anhydrous Na2SO4, concentrated, purified by column chromatography using ethyl acetate/hexane (7:3 v/v).
Activationnone reported
Scalability context1.0 mmol scale; pdiq yield 83% shown in Scheme S1.
Show 5 structured reagent records
RoleReagentAmount / concentrationSource
Linker2-(1H-benzo[d]imidazol-2-yl) aniline209 mg, 1.0 mmolp003 / article p.3140 · Experimental Section - Synthesis of the Ligand (pdiq) · Scheme S1
Linkerisonicotinaldehyde107 mg, 1.0 mmolp003 / article p.3140 · Experimental Section - Synthesis of the Ligand (pdiq) · Scheme S1
Solventethanol10.0 mLp003 / article p.3140 · Experimental Section - Synthesis of the Ligand (pdiq) · Scheme S1
Solventethyl acetate/hexane7:3 v/v eluentp003 / article p.3140 · Experimental Section - Synthesis of the Ligand (pdiq) · Scheme S1
Additiveanhydrous Na2SO4not specifiedp003 / article p.3140 · Experimental Section - Synthesis of the Ligand (pdiq) · Scheme S1