Synthesis evidence

Conjugated Nonplanar Copper-Catecholate Conductive Metal-Organic Frameworks via Contorted Hexabenzocoronene Ligands for Electrical Conduction

Xing G., Liu J., Zhou Y. et al. · Journal of the American Chemical Society · 2023 · 8979-8987

3 structured synthesis routes

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

Complete recipeSource: Both

Route 1: Solvothermal

S9 / p009 · Synthesis of c-HBC-12O-Cu · Scheme S8

Metal precursorsCu(NO3)2.3H2O (38.7 mg, 0.16 mmol) in H2O (2.3 mL)
Linker precursorsc-HBC-12OH (31.7 mg, 0.04 mmol) in DMF (0.2 mL)
SolventsH2O; N,N-dimethylformamide (DMF)
Atmospherenot specified
Temperature85
Time72
Work-upSonicated 10 min; cooled to room temperature; precipitate collected by centrifugation and washed with water, DMF and acetone.
ActivationDried under vacuum for 24 h at room temperature.
Scalability contextPreparative scale reported in tens of milligrams with 96% yield.
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceCu(NO3)2.3H2O38.7 mg, 0.16 mmolS9 / p009 · Synthesis of c-HBC-12O-Cu · Scheme S8
Linkerc-HBC-12OH31.7 mg, 0.04 mmolS9 / p009 · Synthesis of c-HBC-12O-Cu · Scheme S8
SolventH2O2.3 mLS9 / p009 · Synthesis of c-HBC-12O-Cu · Scheme S8
SolventDMF0.2 mLS9 / p009 · Synthesis of c-HBC-12O-Cu · Scheme S8
Complete recipeSource: Both

Route 2: Solvothermal

S8 / p008 · Synthesis of c-HBC-6O-Cu · Scheme S6

Metal precursorsCu(NO3)2.3H2O (9.6 mg, 0.04 mmol) in H2O (2.0 mL)
Linker precursorsc-HBC-6OH (7.0 mg, 0.01 mmol) in DMAc (0.5 mL)
SolventsH2O; N,N-dimethylacetamide (DMAc)
Atmospherenot specified
Temperature85
Time72
Work-upSonicated 10 min; cooled to room temperature; precipitate collected by centrifugation and washed with water, DMF and acetone.
ActivationDried under vacuum for 24 h at room temperature.
Scalability contextPreparative scale reported in milligrams with 78% yield.
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceCu(NO3)2.3H2O9.6 mg, 0.04 mmolS8 / p008 · Synthesis of c-HBC-6O-Cu · Scheme S6
Linkerc-HBC-6OH7.0 mg, 0.01 mmolS8 / p008 · Synthesis of c-HBC-6O-Cu · Scheme S6
SolventH2O2.0 mLS8 / p008 · Synthesis of c-HBC-6O-Cu · Scheme S6
SolventDMAc0.5 mLS8 / p008 · Synthesis of c-HBC-6O-Cu · Scheme S6
Complete recipeSource: Both

Route 3: Solvothermal

S9 / p009 · Synthesis of c-HBC-8O-Cu · Scheme S7

Metal precursorsCu(NO3)2.3H2O (48.3 mg, 0.2 mmol) in H2O (4.6 mL)
Linker precursorsc-HBC-8OH (36.4 mg, 0.05 mmol) in DMF (0.4 mL)
SolventsH2O; N,N-dimethylformamide (DMF)
Atmospherenot specified
Temperature85
Time72
Work-upSonicated 10 min; cooled to room temperature; precipitate collected by centrifugation and washed with water, DMF and acetone.
ActivationDried under vacuum for 24 h at room temperature.
Scalability contextPreparative scale reported in tens of milligrams with 92% yield.
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceCu(NO3)2.3H2O48.3 mg, 0.2 mmolS9 / p009 · Synthesis of c-HBC-8O-Cu · Scheme S7
Linkerc-HBC-8OH36.4 mg, 0.05 mmolS9 / p009 · Synthesis of c-HBC-8O-Cu · Scheme S7
SolventH2O4.6 mLS9 / p009 · Synthesis of c-HBC-8O-Cu · Scheme S7
SolventDMF0.4 mLS9 / p009 · Synthesis of c-HBC-8O-Cu · Scheme S7