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William Dampier

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Reagents:
  • 1-Phenyl-2-nitropropene (P2NP; cas 705-60-2) 1.63 g, 10 mmol;
  • Powdered iron (Fe) 3 g;
  • FeCl3 0.6 g;
  • Hydrochloric acid (HCl 36% aq.) conc. 4 ml;
  • Toluene 15 ml;
  • Water 55 ml;
  • Hydrochloric acid 3N (10.45%) HCl 25 ml;
  • Sodium bicarbonate (NaHCO3);
  • Magnesium sulfate (MgSO4);
Equipment and glassware:
Reaction scheme:
O8UfdzDGSj
Synthesis:
1. A mixture of 1-phenyl-2-nitropropene (P2NP) 1.63 g, 10 mmol, powdered iron 3 g, FeCl3 0.6 g, and hydrochloric acid (HCl 36% aq.) concentrated 4 ml in toluene 5 ml and water 5 ml are stirred vigorously at 75 °C for 18 h in 50 ml flask with reflux condenser.
2. The resulting dark green suspension is cooled to room temperature and filtered. Layers are separated.
3. The aqueous layer is washed with an additional portion of toluene 10 ml, and toluene extracts are combined and
washed with hydrochloric acid 3N (10.45%) HCl 25 ml, water 25 ml, saturated sodium bicarbonate (NaHCO3) aq. 25 ml, and water 25 ml successively to neutral pH 7.
4. The toluene solution is filtered and dried over anhydrous
magnesium sulfate (MgSO4). Mixture is filtered from solids.
5. Toluene solvent is
evaporated from the mixture. Phenyl-2-propanone (P2P; cas 103-79-7) is obtained as an orange oil. The yield is ~75%.
 
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btcboss2022

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Hello,

I tried this synth but is practically impossible to move the magnetic stirrer, all the iron gets stuck on it not allowing to move( is normal about magnet) haahaha how do you fix that?

Thanks.

Reaction scheme:
View attachment 1476

Synthesis:
1. A mixture of 1-phenyl-2-nitropropene (1,63 g, 10 mmol), powdered iron (3 g), FeCl3 (0,6 g), and concentrated HCl (4 ml) in toluene (5 ml) and water (5 ml) was stirred vigorously at 75 *C for 18 h.
2. The resulting dark green suspension was cooled to room temperature and gravity filtered; the layers were allowed to separate.
3. The aqueous layer was washed with an additional portion of toluene (10 ml), and the toluene extracts were combined and washed successively with 3 N HCl (25 ml), water (25 ml), saturated sodium bicarbonate (25 ml), and water (25 ml).
4. The toluene solution was gravity filtered and dried over anhydrous magnesium sulfate.
5. Filtration followed by evaporation of the filtrate solvent yielded phenyl-2-propanone as an orange oil.
 

G.Patton

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Hello,

I tried this synth but is practically impossible to move the magnetic stirrer, all the iron gets stuck on it not allowing to move( is normal about magnet) haahaha how do you fix that?

Thanks.
top stirrer
 

KokosDreams

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Reaction scheme:
View attachment 1476

Synthesis:
1. A mixture of 1-phenyl-2-nitropropene (1,63 g, 10 mmol), powdered iron (3 g), FeCl3 (0,6 g), and concentrated HCl (4 ml) in toluene (5 ml) and water (5 ml) was stirred vigorously at 75 *C for 18 h.
2. The resulting dark green suspension was cooled to room temperature and gravity filtered; the layers were allowed to separate.
3. The aqueous layer was washed with an additional portion of toluene (10 ml), and the toluene extracts were combined and washed successively with 3 N HCl (25 ml), water (25 ml), saturated sodium bicarbonate (25 ml), and water (25 ml).
4. The toluene solution was gravity filtered and dried over anhydrous magnesium sulfate.
5. Filtration followed by evaporation of the filtrate solvent yielded phenyl-2-propanone as an orange oil.

What's the obtained yield in P2P from this synthesis?
@btcboss2022
@G.Patton
 
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