Sodium Hydroxide → HCID 21998681, compound
Reaction equation
[CH:1]12[CH2:7][CH2:6][CH:5]1[CH2:4][C:3](=[O:8])[CH2:2]2.[NH2:9]OS(O)(=O)=O.[OH-].[Na+]>C(O)=O>[O:8]=[C:3]1[CH2:4][CH:5]2[CH:1]([CH2:7][CH2:6]2)[CH2:2][NH:9]1Participants
5
Reactant 3
Product 1
Reagents, catalysts & solvents 1
Procedure
To a solution of 0.48 g of bicyclo[3.2.0]heptan-3-one in 8 ml of formic acid was added 725 mg of hydroxylamine-O-sulfonic acid, followed by heat-refluxing for 3 hours. The reaction mixture was allowed to cool, poured into ice water, neutralized with a 5N sodium hydroxide aqueous solution, and extracted with chloroform. The organic layer was washed, dried, and concentrated under reduced pressure. The residue was purified by silica gel column chromatography to give 48 mg of the title compound as a brown solid, which had the following physical properties.
Workup
- temperatureby heat-refluxing for 3 hours
- temperatureto cool
- extractionextracted with chloroform
- washThe organic layer was washed
- customdried
- concentrationconcentrated under reduced pressure
- customThe residue was purified by silica gel column chromatography
Sources & evidence
- ORD record
- ord-cc2267c4ffdb46388136ebe23dc4c561
- Source dataset
- uspto-grants-2001_05
- Patent number
- US06228866B1
Reaction notes
Loading…