Synthesis evidence

Two-dimensional π-conjugated metal-organic framework with high electrical conductivity for electrochemical sensing

Wu F., Fang W., Yang X. et al. · Journal of the Chinese Chemical Society · 2019 · 522-528

3 structured synthesis routes

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

Partial recipeSource: Main

Route 1: Drop Cast

p003 (journal p.524) · 2.4 Preparation of the Cu3(HHTP)2/GCE

Solventswater suspension of Cu3(HHTP)2; ethanol and deionized water used for rinsing
Additives0.3- and 0.05-um Al2O3 polishing powder
Atmospheredried in N2 during GCE cleaning; final drop-cast dried at room temperature
Temperatureroom temperature
Time5
Substrate orientationglassy carbon electrode surface
Work-upPolished GCE with Al2O3 powder, rinsed in ethanol and deionized water, dried in N2; dropped 5 uL Cu3(HHTP)2 aqueous suspension onto clean GCE surface; dried at room temperature for 5 h.
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
OtherCu3(HHTP)2 suspension in water5 uL · not reportedp003 (journal p.524) · 2.4 Preparation of the Cu3(HHTP)2/GCE
Solventethanolrinsep003 (journal p.524) · 2.4 Preparation of the Cu3(HHTP)2/GCE
Solventdeionized waterrinse and suspension mediump003 (journal p.524) · 2.4 Preparation of the Cu3(HHTP)2/GCE
AdditiveAl2O3 powder0.3- and 0.05-um polishing powderp003 (journal p.524) · 2.4 Preparation of the Cu3(HHTP)2/GCE
Vague recipeSource: Main

Route 2: Drop Cast

p003 (journal p.524) · 3.1 Characterization of Cu3(HHTP)2 · Figure 1b

Solventswater suspension of Cu3(HHTP)2
Atmospherenot specified
Substrate orientationITO-coated glass
Work-upDrop-cast Cu3(HHTP)2 suspension in water onto ITO-coated glass.
Scalability contextDescribed as a simple and robust electrode-modification method.
Show 1 structured reagent record
RoleReagentAmount / concentrationSource
OtherCu3(HHTP)2 suspension in waternot reported · not reportedp003 (journal p.524) · 3.1 Characterization of Cu3(HHTP)2 · Figure 1b
Complete recipeSource: Main

Route 3: Solvothermal

p002 (journal p.523) · 2.3 Synthesis and activation of the Cu3(HHTP)2

Metal precursorsCuNO3*3H2O, 10 mg (raw source text; likely intended copper nitrate hydrate)
Linker precursorsHHTP, 7 mg
Solvents1.5 mL deionized water; 0.165 mL 1-methyl-2-pyrrolidinone (NMP)
Atmospherenot specified
Temperature85
Time24
Work-upCooled naturally to room temperature; centrifuged three cycles at 10000 rpm for 6 min with washing; washed with deionized water (3 x 3 mL) and acetone (6 x 3 mL); dried in air.
ActivationSolvent exchange with acetone refreshed three times for 1 week; evacuated at room temperature for 10 h; heated at 85 C for 24 h to remove acetone.
Scalability contextSmall vial synthesis: 5 mL glass vial, milligram reagent quantities.
Show 5 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceCuNO3*3H2O10 mgp002 (journal p.523) · 2.3 Synthesis and activation of the Cu3(HHTP)2
LinkerHHTP7 mgp002 (journal p.523) · 2.3 Synthesis and activation of the Cu3(HHTP)2
Solventdeionized water1.5 mLp002 (journal p.523) · 2.3 Synthesis and activation of the Cu3(HHTP)2
Solvent1-methyl-2-pyrrolidinone (NMP)0.165 mLp002 (journal p.523) · 2.3 Synthesis and activation of the Cu3(HHTP)2
Solventacetone6 x 3 mL wash; refreshed three times for 1 week during activationp002 (journal p.523) · 2.3 Synthesis and activation of the Cu3(HHTP)2