Phosphoric Acid → 1-(5-Ethylthiophen-2-yl)ethan-1-one
Reaction equation
[CH2:1]([C:3]1[S:4][CH:5]=[CH:6][CH:7]=1)[CH3:2].P(=O)(O)(O)O.C(O[C:17](=[O:19])[CH3:18])(=O)C>>[CH2:1]([C:3]1[S:4][C:5]([C:17](=[O:19])[CH3:18])=[CH:6][CH:7]=1)[CH3:2]Participants
4
Conditions
- Temperature
- 80 °C
Procedure
In a 50 ml three-necked flask, 5 g (44.6 mmol, 1 eq) of 2-ethylthiophene are dissolved in 28 ml of acetic anhydride, 0.5 ml of ortho-phosphoric acid are added and the reaction mixture is then heated for 1 hour at 80° C. The acids are evaporated off under reduced pressure, and the oil obtained is then filtered over a silica patch (eluent: 20% ethyl acetate, 80% heptane) after evaporation of the solvents: 5.2 g of 1-(5-ethylthiophen-2-yl)ethanone are obtained in the form of a brown oil. Yield: 76%.
Workup
- customThe acids are evaporated off under reduced pressure
- customthe oil obtained
- filtrationis then filtered over a silica patch (eluent: 20% ethyl acetate, 80% heptane)
- customafter evaporation of the solvents
Sources & evidence
- ORD record
- ord-04884c5c5d604af49568ebd43bb6e177
- Source dataset
- uspto-grants-2011_08
- Patent number
- US07989483B2
Reaction notes
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