Hydrogen iodide → HCID 70979807, compound
Reaction equation
[CH3:1][CH:2]([CH:6]([C:9]1[CH:14]=[CH:13][CH:12]=[C:11]([O:15]C)[CH:10]=1)[CH2:7][CH3:8])[C:3]([OH:5])=[O:4].I>>[CH3:1][CH:2]([CH:6]([C:9]1[CH:14]=[CH:13][CH:12]=[C:11]([OH:15])[CH:10]=1)[CH2:7][CH3:8])[C:3]([OH:5])=[O:4]Participants
3
Procedure
The steps are: add 2-methyl-3-(3-methoxyphenyl) valeric acid into a reaction flask, add hydroiodic acid, and perform heating and reflux for 12 hours; detect the reaction process by TLC; after that, cool the resultant to the room temperature, pour it into an alkaline solution to make the pH become 9, perform extraction by ethyl acetate, reversely adjust the pH of the water layer to about 3.0 after the water layer is separated out, and add ethyl acetate for extraction; and dry the ethyl acetate extracting solution by anhydrous magnesium sulphate, and recycle the solvent by decompression to obtain a light yellow liquid, 2-methyl-3-(3-hydroxyphenyl) valeric acid.
Workup
- temperatureperform heating
- temperaturereflux for 12 hours
- additionpour it into an alkaline solution
- extractionextraction by ethyl acetate
- customis separated out
- additionadd ethyl acetate
- extractionfor extraction
- dry with materialand dry the ethyl acetate extracting solution by anhydrous magnesium sulphate
Sources & evidence
- ORD record
- ord-7a96d4f8385d4b49ad43f25fe5449d0d
- Source dataset
- uspto-grants-2014_10
- Patent number
- US08853393B2
Reaction notes
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