Hydrochloric Acid → HCID 58460122, compound
Reaction equation
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]([NH:10][NH:11][C:12]([NH:14][CH2:15][C:16]([O:18]CC)=[O:17])=[O:13])=O)=[CH:4][CH:3]=1.[OH-].[Na+].Cl>>[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[N:14]([CH2:15][C:16]([OH:18])=[O:17])[C:12](=[O:13])[NH:11][N:10]=2)=[CH:4][CH:3]=1Participants
4
Procedure
Of the compound from Example 1A, 21.43 g (67.93 mmol) were admixed with 91 ml of a 3N aqueous sodium hydroxide solution and heated at reflux overnight. After cooling to RT, the mixture was adjusted to a pH of 1 by slow addition of approximately 20% strength hydrochloric acid. The precipitated solid was isolated by filtration, washed with water and dried at 60° C. under reduced pressure. Yield: 17.55 g (90% of theory, approximately 88% purity).
Workup
- temperatureheated
- temperatureat reflux overnight
- customThe precipitated solid was isolated by filtration
- washwashed with water
- customdried at 60° C. under reduced pressure
Sources & evidence
- ORD record
- ord-af6d146423c74108b6eafd0d4e4cda82
- Source dataset
- uspto-grants-2012_06
- Patent number
- US08202895B2
Reaction notes
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