Synthesis evidence

A Mixed Heterobimetallic Y/Eu-MOF for the Cyanosilylation and Hydroboration of Carbonyls

Echenique-Errandonea E., Lopez-Vargas M.E., Perez J.M. et al. · Catalysts · 2022 · 299

2 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

7 · 3.2 Synthesis of Catalyst and General Procedures of Catalysis

Metal precursorsEu(NO3)3.5H2O (0.006 g, 0.0145 mmol); Y(NO3)3.6H2O (0.011 g, 0.0289 mmol)
Linker precursors3-amino-4-hydroxybenzoic acid (0.010 g, 0.0625 mmol)
SolventsDMF and distilled water
AdditivesEt3N (10 uL, 0.072 mmol)
Atmospherenot specified for MOF synthesis
Temperature100
Time2
Work-upMetal solution was added dropwise under continuous agitation to ligand solution; brown solution heated in screw-capped 6 mL vial to yield hexagonal single crystals.
Activationnot specified; formula retains coordinated water and 12 DMF molecules
Scalability contextSI provides a larger-scale variant with 0.2 g linker and 83 mg isolated product.
Show 6 structured reagent records
RoleReagentAmount / concentrationSource
Linker3-amino-4-hydroxybenzoic acid0.010 g, 0.0625 mmol7 · 3.2 Synthesis of Catalyst and General Procedures of Catalysis
SolventDMF0.2 mL initially plus 0.2 mL added to metal solution7 · 3.2 Synthesis of Catalyst and General Procedures of Catalysis
BaseEt3N10 uL, 0.072 mmol7 · 3.2 Synthesis of Catalyst and General Procedures of Catalysis
Metal SourceEu(NO3)3.5H2O0.006 g, 0.0145 mmol7 · 3.2 Synthesis of Catalyst and General Procedures of Catalysis
Metal SourceY(NO3)3.6H2O0.011 g, 0.0289 mmol7 · 3.2 Synthesis of Catalyst and General Procedures of Catalysis
Solventdistilled water0.8 mL initially plus 0.8 mL added to ligand solution7 · 3.2 Synthesis of Catalyst and General Procedures of Catalysis
Complete recipeSource: SI

Route 2: Solvothermal

S6 · 2. General procedures

Metal precursorsEu(NO3)3.5H2O (0.124 g, 0.289 mmol); Y(NO3)3.6H2O (0.221 g, 0.578 mmol)
Linker precursors3-amino-4-hydroxybenzoic acid (0.2 g, 1.2 mmol)
SolventsDMF/H2O solvent mixture and water
AdditivesEt3N (200 uL, 1.44 mmol)
Atmospherenot specified for MOF synthesis
Temperature100
Time2
Work-upMetal mixture in water added dropwise under magnetic agitation; brownish precipitate redissolved; heated in oven; single crystalline product obtained.
Activationnot specified; PXRD used to confirm purity
Scalability contextScale-up synthesis gave 83 mg heterobimetallic Y/Eu-MOF.
Show 6 structured reagent records
RoleReagentAmount / concentrationSource
Linker3-amino-4-hydroxybenzoic acid0.2 g, 1.2 mmolS6 · 2. General procedures
SolventDMF/H2O solvent-mixture1.2/3 mLS6 · 2. General procedures
BaseEt3N200 uL, 1.44 mmolS6 · 2. General procedures
Metal SourceEu(NO3)3.5H2O0.124 g, 0.289 mmolS6 · 2. General procedures
Metal SourceY(NO3)3.6H2O0.221 g, 0.578 mmolS6 · 2. General procedures
Solventwater1.8 mLS6 · 2. General procedures