1,4-Dioxane hydrochloride → HCID 66990698, compound
Reaction equation
[ClH:1].O1CCOCC1.[OH:8][C:9]1[CH:38]=[CH:37][C:36]([N:39]2[CH2:44][CH2:43][CH2:42][CH2:41][CH2:40]2)=[CH:35][C:10]=1[C:11]([NH:13][C:14]1[CH:26]=[C:25]([C:27]2[CH:32]=[CH:31][CH:30]=[CH:29][C:28]=2[O:33][CH3:34])[CH:24]=[CH:23][C:15]=1[C:16]([O:18]C(C)(C)C)=[O:17])=[O:12]>>[ClH:1].[OH:8][C:9]1[CH:38]=[CH:37][C:36]([N:39]2[CH2:44][CH2:43][CH2:42][CH2:41][CH2:40]2)=[CH:35][C:10]=1[C:11]([NH:13][C:14]1[CH:26]=[C:25]([C:27]2[CH:32]=[CH:31][CH:30]=[CH:29][C:28]=2[O:33][CH3:34])[CH:24]=[CH:23][C:15]=1[C:16]([OH:18])=[O:17])=[O:12]Participants
3
Procedure
A 4 mol/L hydrogen chloride-dioxane solution (3.0 mL) was added to the obtained tert-butyl 2-(2-hydroxy-5-(piperidin-1-yl)benzamido)-4-(2-methoxyphenyl)benzoate (0.025 g), followed by stirring at room temperature for 3 hours and then at 50 to 55° C. for 1 hour. The reaction mixture was cooled to room temperature, and then the solvent was evaporated under reduced pressure. Diisopropyl ether was added to the obtained residue, and the solid substance was collected by filtration to obtain 0.020 g of 2-(2-hydroxy-5-(piperidin-1-yl)benzamido)-4-(2-methoxyphenyl)benzoic acid hydrochloride as a white solid.
Workup
- waitat 50 to 55° C. for 1 hour
- temperatureThe reaction mixture was cooled to room temperature
- customthe solvent was evaporated under reduced pressure
- additionDiisopropyl ether was added to the obtained residue
- filtrationthe solid substance was collected by filtration
Sources & evidence
- ORD record
- ord-665433e844064887aef537a87a3934e9
- Source dataset
- uspto-grants-2013_07
- Patent number
- US08492582B2
Reaction notes
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