Sodium Carbonate → HCID 118162236, compound
Reaction equation
[OH:1][CH:2]1[CH2:7][CH2:6][CH2:5][C:4](=O)[C:3]1([CH3:10])[CH3:9].Cl.[NH2:12][OH:13].C(=O)([O-])[O-].[Na+].[Na+]>CCO.O>[OH:1][CH:2]1[CH2:7][CH2:6][CH2:5][C:4](=[N:12][OH:13])[C:3]1([CH3:10])[CH3:9]Participants
6
Conditions
- Temperature
- 25 °C
Procedure
A mixture of 3-hydroxy-2,2-dimethylcyclohexanone (1.6 g, crude), hydroxylamine hydrochloride (2.98 g, 42.9 mmol) and sodium carbonate (4.54 g, 42.9 mmol) in EtOH (30 mL) and water (3 mL) was stirred at 25° C. for 6 h. The organic solvents were removed under reduced pressure and the residue was extracted with ethyl acetate (2×200 mL). The combined organic layers were washed with brine, dried over anhydrous sodium sulfate and concentrated to afford the title compound (1.8 g, crude). MS (ESI) m/z 158.2 [M+H]+.
Workup
- customThe organic solvents were removed under reduced pressure
- extractionthe residue was extracted with ethyl acetate (2×200 mL)
- washThe combined organic layers were washed with brine
- dry with materialdried over anhydrous sodium sulfate
- concentrationconcentrated
Sources & evidence
- ORD record
- ord-3bd1596ba3a2444e8f197b7db9cbe60c
- Source dataset
- uspto-grants-2015_10
- Patent number
- US09156798B2
Reaction notes
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