Metal precursorsanhydrous FeCl3 (Sinopharm), 114 mg, 0.7 mmol, 5% excess
Linker precursors2,5-dihydroxy-1,4-benzoquinone (DHBQ, Alfa Aesar), 140 mg, 1.0 mmol
Solvents20 mL deionized water; 20 mL ethanol; H2O/EtOH volume ratio 1:1 during final reflux
Atmosphereair atmosphere for DHBQ/Fe(OH)3 reflux; stored in air several hours after drying
Temperature88 C azeotropic reflux for H2O/EtOH mixture; 80 C vacuum drying
TimeFeCl3 aqueous reflux 10 min; final reflux 1 h; vacuum dry 12 h; air storage several hours
Oxidant / reductantFeCl3 as Fe3+ source; oxidative air atmosphere; Fe(OH)3 weak base deprotonates DHBQ
Work-upCool to room temperature; centrifuge precipitate; wash with deionized water three times and ethanol three times.
ActivationVacuum drying at 80 C for 12 h; air equilibration to stable Fe2(C6H2O4)3.2H2O.
Scalability contextAuthors describe the synthesis as easy and low cost; isolated yield 93% based on Fe2(C6H2O4)3.2H2O.
Show 4 structured reagent records
| Role | Reagent | Amount / concentration | Source |
|---|
| Metal Source | anhydrous FeCl3 (Sinopharm) | 114 mg (0.7 mmol, 5% excess) | 432 · 4.1. Material synthesis |
| Linker | 2,5-dihydroxy-1,4-benzoquinone (DHBQ, Alfa Aesar) | 140 mg (1.0 mmol) | 432 · 4.1. Material synthesis |
| Solvent | deionized water | 20 mL | 432 · 4.1. Material synthesis |
| Solvent | ethanol | 20 mL | 432 · 4.1. Material synthesis |