Iodine → HCID 20303480, compound
Reaction equation
II.[Cl:3][C:4]1[CH:5]=[N:6][N:7]([C:9]2[CH:19]=[CH:18][C:12]([CH:13](O)[C:14]([OH:16])=[O:15])=[CH:11][CH:10]=2)[CH:8]=1>C(O)(=O)C>[Cl:3][C:4]1[CH:5]=[N:6][N:7]([C:9]2[CH:10]=[CH:11][C:12]([CH2:13][C:14]([OH:16])=[O:15])=[CH:18][CH:19]=2)[CH:8]=1Participants
4
Reactant 2
Product 1
Reagents, catalysts & solvents 1
Procedure
340 mg of red phosphorus and 110 mg of iodine are added to 10 ml of glacial acetic acid. After 15 minutes, 2.8 g (0.01 mole) of 4-(4-chloropyrazol-1-yl) mandelic acid are added; heating under reflux is effected for 4 hours, followed by cooling, filtration, pouring on to a sodium sulphite solution and extraction with ether. The ethereal solution is dried and concentrated. 4-(4-chloropyrazol-1-yl) phenylacetic acid (m.p. 176°-178° C.) is obtained.
Workup
- temperatureheating
- temperatureunder reflux
- waitis effected for 4 hours
- temperatureby cooling
- filtrationfiltration
- additionpouring on to a sodium sulphite solution and extraction with ether
- customThe ethereal solution is dried
- concentrationconcentrated
Sources & evidence
- ORD record
- ord-337b8e1eabf84b39b0734e57ce9be14e
- Source dataset
- uspto-grants-1980_12
- Patent number
- US04239901
Reaction notes
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