cMOF Evidence Base

Synthesis evidence

Two-Dimensional Conductive Metal-Organic Frameworks Based on Truxene

Zhao Q., Li S.-H., Chai R.-L. et al. · ACS Applied Materials and Interfaces · 2020 · 7504-7509

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: Drop Cast

S-20 · Electrical properties of the MOF · Figure 4

Solventswater (0.5 mL) and isopropanol (0.5 mL)
Atmospheredried at room temperature; GC preparation dried in N2 atmosphere
Temperatureroom temperature
Time3
Substrate orientation5 uL suspension dropped onto polished GC electrode surface
Work-upGC polished with Al2O3 powders, rinsed with ethanol and water, activated by CV scans in sulfuric acid, ultrasonically washed, dried in N2; cMOF suspension drop-cast and dried.
Scalability contextSmall-volume electrode modification for a 3 mm diameter GC working electrode.
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
Othertruxene-Cu MOF1.0 mg; 5 uL suspension used · 1.0 mg in 1.0 mL total water/isopropanolS-20 · Electrical properties of the MOF · Figure 4
Solventwater0.5 mLS-20 · Electrical properties of the MOF · Figure 4
Solventisopropanol0.5 mLS-20 · Electrical properties of the MOF · Figure 4
OtherAl2O3 polishing powders1.5 um, 500 nm, and 50 nm powdersS-20 · Electrical properties of the MOF · Figure 4
Complete recipeSource: Both

Route 2: Other

7507 · Experimental Section · Scheme S1; Figures S1-S3

Linker precursors2,3,7,8,12,13-hexamethoxy-truxene reddish solid (1.0 g, 1 equiv)
SolventsCH2Cl2 (40 mL plus 10 mL BBr3 solution); water quench; CH2Cl2, H2O, acetone washes
Atmospherenot stated
Temperature0 then room temperature
Time2 h at room temperature plus 30 min after water quench
Oxidant / reductantBBr3 (1 mL, 5.6 equiv) as demethylating Lewis acid
Work-upWater added to quench; precipitate collected and washed with CH2Cl2 (20 mL), H2O (20 mL), and acetone (5 mL).
ActivationSubjected to 1H NMR, 13C NMR, and HRMS.
Scalability context1.0 g intermediate scale; grey powder product yield 52%.
Show 5 structured reagent records
RoleReagentAmount / concentrationSource
Linker2,3,7,8,12,13-hexamethoxy-truxene1.0 g, 1 equiv7507 · Experimental Section · Scheme S1; Figures S1-S3
SolventCH2Cl240 mL plus 10 mL7507 · Experimental Section · Scheme S1; Figures S1-S3
AcidBBr31 mL, 5.6 equiv7507 · Experimental Section · Scheme S1; Figures S1-S3
SolventH2Oquench plus 20 mL wash7507 · Experimental Section · Scheme S1; Figures S1-S3
Solventacetone5 mL wash7507 · Experimental Section · Scheme S1; Figures S1-S3
Complete recipeSource: Both

Route 3: Other

7507 · Experimental Section · Scheme S1

Linker precursors5,6-dimethoxy-1-indanone (2.0 g)
Solventspolyphosphoric ester (20 mL); CHCl3 and EtOH dilution; CHCl3 and acetone washes
Additivespolyphosphoric ester
Atmospherenot stated
Temperature150
Timeovernight
Work-upAfter cooling, diluted with CHCl3 and EtOH; precipitate collected and washed with CHCl3 (20 mL) and acetone (20 mL).
ActivationUsed crude in next step without further purification.
Scalability context2.0 g precursor scale; crude yield 41%; product was insoluble in common laboratory solvents.
Show 5 structured reagent records
RoleReagentAmount / concentrationSource
Linker5,6-Dimethoxy-1-indanone2.0 g7507 · Experimental Section · Scheme S1
Additivepolyphosphoric ester20 mL7507 · Experimental Section · Scheme S1
SolventCHCl320 mL wash; additional dilution amount not stated7507 · Experimental Section · Scheme S1
SolventEtOHdilution amount not stated7507 · Experimental Section · Scheme S1
Solventacetone20 mL wash7507 · Experimental Section · Scheme S1
Complete recipeSource: Both

Route 4: Liquid Liquid Interface

7507 · Experimental Section · Figure 1a; Figure S4

Metal precursorsCu(OAc)2 (27.2 mg, 1.5 equiv) dissolved in 100 mL water
Linker precursors2,3,7,8,12,13-hexahydroxyl truxene (43.8 mg, 1 equiv) dissolved in 100 mL ethyl acetate
Solventsethyl acetate (EA, 100 mL plus EA washes); water (100 mL plus H2O washes); acetone washes
Atmosphereair/not stated; biphasic mixture left undisturbed
Temperatureroom temperature
Time24
Substrate orientationEA organic phase carefully layered onto aqueous Cu(OAc)2 phase
Oxidant / reductantCu(II) acetate; redox state evolves to mixed Cu(I)/Cu(II) in product
Work-upOrganic layer removed; interfacial film collected; washed with H2O (5 mL x 3), EA (5 mL x 3), and acetone (5 mL x 3); centrifuged to isolate black powder.
ActivationEvacuated at room temperature for 10 h followed by heating at 85 deg C for 24 h to remove acetone.
Scalability context100 mL/100 mL liquid-liquid interface; product yield 77%. SI Figure S4 shows a black interfacial solid after 12 h, whereas the main recipe leaves the biphasic mixture for 1 day.
Show 5 structured reagent records
RoleReagentAmount / concentrationSource
Linker2,3,7,8,12,13-hexahydroxyl truxene43.8 mg, 1 equiv · in 100 mL EA7507 · Experimental Section · Figure 1a; Figure S4
Metal SourceCu(OAc)227.2 mg, 1.5 equiv · in 100 mL water7507 · Experimental Section · Figure 1a; Figure S4
Solventethyl acetate (EA)100 mL plus 5 mL x 3 wash7507 · Experimental Section · Figure 1a; Figure S4
Solventwater100 mL plus 5 mL x 3 wash7507 · Experimental Section · Figure 1a; Figure S4
Solventacetone5 mL x 3 wash7507 · Experimental Section · Figure 1a; Figure S4