116174-33-5 → 857995-47-2
Reaction equation
[CH3:1][S:2][C:3]1[CH:8]=[CH:7][C:6]([CH2:9][CH2:10][CH2:11][C:12]([OH:14])=O)=[CH:5][CH:4]=1>O>[CH3:1][S:2][C:3]1[CH:4]=[C:5]2[C:6]([CH2:9][CH2:10][CH2:11][C:12]2=[O:14])=[CH:7][CH:8]=1Participants
3
Reactant 1
Product 1
Reagents, catalysts & solvents 1
Conditions
- Temperature
- 60 °C
Procedure
0.055 mol of the compound obtained in Step B and 100 g of polyphosphoric acid are introduced into a 500 ml round-bottomed flask. The reaction mixture is heated at 60° C. for 3 hours and is then cooled and poured into water. Extraction with ethyl ether is carried out; the organic phase is washed with water, dried over MgSO4 and evaporated under reduced pressure. The residue obtained is purified by chromatography on silica gel. Yellow oil
Workup
- temperatureis then cooled
- extractionExtraction with ethyl ether
- washthe organic phase is washed with water
- dry with materialdried over MgSO4
- customevaporated under reduced pressure
- customThe residue obtained
- customis purified by chromatography on silica gel
Sources & evidence
- ORD record
- ord-f3fca84a6e1e42789dade9da8fbd7fc9
- Source dataset
- uspto-grants-2006_10
- Patent number
- US07126012B2
Reaction notes
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