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FriendlyFinger
(Hive Bee)
11-08-02 06:25
No 377568
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I want to make proipiophenone
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Howdy!
From my recent experience, propiophenone is hard to find. So is propionyl chloride but propionic acid is no problem. TFSE said I can use propionic acid and polyphosphoric acid and to look up PIHKAL, so I did. This is what I found first;
#71 DOPR
There was added a solution of 74 g 2,5-dimethoxypropiophenone (from the reaction of propionic acid and p-dimethoxybenzene in the presence of polyphosphoric acid, see under DOAM for an effective general procedure) in 140 g EtOH.
Next I found this; #61 DOAM
A solution of 110 g p-dimethoxybenzene and 102 g valeric acid in 168 g polyphosphoric acid was heated on the steam bath for 3 h, giving a deep red homogeneous solution. This was poured into 1 L H2O with good stirring. The strongly acidic, cloudy suspension was extracted with 3x200 mL CH2Cl2, the extracts pooled, washed with 4x150 mL 5% NaOH, and finally once with dilute HCl. The solvent was removed under vacuum, and the residual amber oil cooled overnight at 0 °C. Some 30 g of crystalline, unreacted dimethoxybenzene were removed by filtration, and the 85 g of residual oil distilled at the water pump. Another 15 g of di-methoxybenzene came over as an early cut, but the fraction boil-ing at 184-192 °C (mostly 188-192 °C) weighed 53.0 g and was reasonably pure 2,5-dimethoxyamylophenone.
Does this mean that I can use an equal mole amount of propionic acid instead of valeric acid?
Thanks, FF
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Rhodium
(Chief Bee)
11-08-02 06:42
No 377575
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Yup, exactly.
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Antoncho
(Official Hive Translator)
11-08-02 10:35
No 377622
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Pardon me, sirs....
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....but are you talking of plain or substituted propiophenone?
Cause i really doubt that plain propiophenone can bee made like this - just in case.
Antoncho
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Rhodium
(Chief Bee)
11-08-02 11:56
No 377636
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../rhodium/acetophenones.
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