Phosphorus oxychloride → HCID 178489920, compound
Reaction equation
[F:1][C:2]1[CH:7]=[CH:6][C:5]([CH:8]([C:12]2[NH:16][C:15](/[CH:17]=[CH:18]/[C:19]3[CH:24]=[CH:23][C:22]([N:25]4[CH:29]=[C:28]([CH3:30])[N:27]=[CH:26]4)=[C:21]([O:31][CH3:32])[CH:20]=3)=[N:14][N:13]=2)[CH2:9][CH2:10]O)=[CH:4][CH:3]=1.P(Cl)(Cl)([Cl:35])=O>>[Cl:35][CH2:10][CH2:9][CH:8]([C:12]1[NH:16][C:15](/[CH:17]=[CH:18]/[C:19]2[CH:24]=[CH:23][C:22]([N:25]3[CH:29]=[C:28]([CH3:30])[N:27]=[CH:26]3)=[C:21]([O:31][CH3:32])[CH:20]=2)=[N:14][N:13]=1)[C:5]1[CH:6]=[CH:7][C:2]([F:1])=[CH:3][CH:4]=1Participants
3
Procedure
A solution of 3-(4-fluorophenyl)-3-{5-{(E)-2-[3-methoxy-4-(4-methyl-1H-imidazol-1-yl)phenyl]vinyl}-4H-[1,2,4]triazol-3-yl}propan-1-ol (83 mg) in phosphorus oxychloride (1 mL) was stirred at 120° C. for one hour. The reaction solution was left to cool to room temperature and then concentrated under reduced pressure. Ethyl acetate and saturated sodium bicarbonate water were added to the residue, and the organic layer was separated. The resulting organic layer was dried over anhydrous magnesium sulfate and concentrated under reduced pressure to obtain 86 mg of the title compound. The property value of the compound is as follows.
Workup
- waitThe reaction solution was left
- concentrationconcentrated under reduced pressure
- additionEthyl acetate and saturated sodium bicarbonate water were added to the residue
- customthe organic layer was separated
- dry with materialThe resulting organic layer was dried over anhydrous magnesium sulfate
- concentrationconcentrated under reduced pressure
Sources & evidence
- ORD record
- ord-d99dbc4ee5054495977630087d9422cf
- Source dataset
- uspto-grants-2011_03
- Patent number
- US07897632B2
Reaction notes
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