Complete recipeSource: Main
Route 1: Other
20815 · Methods - Preparation of (NBu4)2Fe2(DHBQ)3 · Figure 1a
Metal precursorsFeSO4.7H2O (0.28 g, 1.00 mmol) dissolved in 10 mL degassed water
Linker precursorsDHBQ (0.21 g, 1.50 mmol)
Solventsdegassed water: 50 mL for DHBQ/NBu4Br dispersion plus 10 mL for FeSO4.7H2O solution
Additivesexcess tetrabutylammonium bromide (NBu4Br, 4.00 g)
AtmosphereAr atmosphere; degassed water; three-necked flask
Temperaturereflux; dried at 80 C
Time2 h reflux after FeSO4.7H2O addition; 10 h vacuum drying
Oxidant / reductantIn situ Fe2+ to Fe3+ oxidation and DHBQ2- to DHBQ3- reduction described by authors.
Work-upCool to room temperature; collect solid by vacuum filtration; thoroughly wash with degassed water.
ActivationDried at 80 C in a vacuum oven for 10 h.
Scalability contextYield: brown solid, 0.35 g, 69.31%.
Show 4 structured reagent records
| Role | Reagent | Amount / concentration | Source |
|---|---|---|---|
| Metal Source | FeSO4.7H2O | 0.28 g, 1.00 mmol · in 10 mL degassed water | 20815 · Methods - Preparation of (NBu4)2Fe2(DHBQ)3 · Figure 1a |
| Linker | DHBQ | 0.21 g, 1.50 mmol · dispersed in 50 mL degassed water | 20815 · Methods - Preparation of (NBu4)2Fe2(DHBQ)3 · Figure 1a |
| Additive | NBu4Br | 4.00 g, excessive · dispersed with DHBQ | 20815 · Methods - Preparation of (NBu4)2Fe2(DHBQ)3 · Figure 1a |
| Solvent | degassed water | 50 mL plus 10 mL | 20815 · Methods - Preparation of (NBu4)2Fe2(DHBQ)3 · Figure 1a |