deadrush
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Clayfen synthesis (iron III nitrate + mort)
First, I presume reacting pure Iron III oxide with dilute nitric acid would yield the same as iron powder and conc. nitric acid?
Second, to make clayfen, do I just mix vigorously the FeNO3 solution and the clay powder? I'd obviously dehydrate it after that but I feel as though
im missing something.
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Texium
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Thread Moved
5-2-2025 at 11:16 |
bnull
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Quote: Originally posted by deadrush  | | to make clayfen, do I just mix vigorously the FeNO3 solution and the clay powder? I'd obviously dehydrate it after that but I feel as though im
missing something. |
The entry in EROS for clayfen: Iron(III) Nitrate–K10 Montmorillonite Clay.
The preparation: | Quote: | Clay-Supported Iron(lll) Nitrate (Clayfen)
Iron(III) nitrate nonahydrate (22.5 g) is added to acetone (375 ml) in a 1 liter, pear-shaped evaporating flask. The mixture is stirred vigorously for
~5 min until complete dissolution of the crystals of hydrated iron(lll) nitrate. The first-formed homogenous rusty brown solution turns after a short
time into a muddy, light brown suspension. K10 clay (30 g) is added in small amounts and stirring is continued for another 5 min. The solvent is then
removed from the resulting suspension under reduced pressure (rotary evaporator) on a water bath at 50 °C. After 30 min, the dry solid crust adhering
to the walls of the flask is flaked off and crushed with a spatula, and rotary evaporator drying is resumed for another 30 min. This procedure yields
KI0 clay-supported iron(lll) nitrate (clayfen) as a yellow, floury powder; yield: ~50g.
Warnings:
- Prolonged heating, or use of a bath temperature > 50 °C, may yield an unstable reagent, which decomposes in a vigorous
exothermic reaction, with emission of a large amount of nitrogen dioxide fumes. This decomposition generally takes place within 15 min after the end
of an incorrect preparation of clayfen.
- Preparation of clayfen includes flaking off of the dry solid crust formed in the evaporator. The physical state of the reagent at this step is
crucial: if this removal is performed w hile the solid is still a little muddy, it will aggregate in spheres that remain wet inside, and the resulting
reagent will display little or no activity, or will decompose as described above. This difficulty will be best avoided by strict observance of the
experimental conditions described (quantities, flask volume and shape).
- Clayfen, spontaneously, slowly loses nitrous fumes, and should never he stored in a closed flask.
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The original publication about clayfen: A. Cornelis, P. Laszlo, Clay-Supported Copper(II) and Iron(III) Nitrates: Novel Multi-Purpose Reagents for
Organic Synthesis, Synthesis 1985; 1985(10): 909-918. https://www.thieme-connect.de/products/ejournals/abstract/10...
Only use the fresh stuff.
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deadrush
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Thank you so much!
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bnull
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Check out your U2Us.
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