Hydrochloric Acid → HCID 675281, compound
Reaction equation
[CH3:1][C:2]1[CH:7]=[CH:6][C:5]([C:8](=O)[CH:9]([CH3:11])[CH3:10])=[CH:4][CH:3]=1.Cl.[NH2:14][OH:15].[OH-].[Na+].Cl>O.C(O)C>[CH3:1][C:2]1[CH:7]=[CH:6][C:5]([C:8](=[N:14][OH:15])[CH:9]([CH3:11])[CH3:10])=[CH:4][CH:3]=1Participants
7
Procedure
3.2 g of 5A, 7.4 g of hydroxylamine hydrochloride, 40 ml of ethanol and 80 ml of water were mixed. 4.4 g of sodium hydroxide was added to the stirred mixture at room temperature. The mixture was stirred for 4 hours at reflux temperature, cooled, poured into cold dilute hydrochloric acid and extracted with methylene chloride. The extract was dried (MgSO4) and stripped of solvent and the product was chromatographed (silica gel, methylene chloride/ether) to give 1-(4-methylphenyl)-2-methyl-1-propanone oxime (5B), as a liquid, boiling point not determined.
Workup
- temperatureat reflux temperature
- temperaturecooled
- extractionextracted with methylene chloride
- dry with materialThe extract was dried (MgSO4)
- customthe product was chromatographed (silica gel, methylene chloride/ether)
Sources & evidence
- ORD record
- ord-66194dc0deaa45e78c643d517f9030f0
- Source dataset
- uspto-grants-1978_03
- Patent number
- US04079149
Reaction notes
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