Sulfuric Acid → HCID 85552580, compound
Reaction equation
[C:1]([C:5]([C:7]1[CH:12]=[CH:11][C:10]([Cl:13])=[CH:9][CH:8]=1)=O)([CH3:4])([CH3:3])[CH3:2].[CH3:14][NH:15][NH2:16].S(=O)(=O)(O)O>C(O)C>[CH3:14][NH:15][N:16]=[C:5]([C:1]([CH3:4])([CH3:3])[CH3:2])[C:7]1[CH:12]=[CH:11][C:10]([Cl:13])=[CH:9][CH:8]=1Participants
5
Reactant 3
Product 1
Reagents, catalysts & solvents 1
Procedure
29.5 g ofg 4-chlorophenyl tert.-butyl ketone (0.15 mol) in 750 ml ethanol was heated under reflux with an excess (118 ml) of methl hydrazine and 3 ml of concentrated sulphuric acid for 4.5 hours. It was concentrated almost to dryness and the added to water. After extraction with methylene chloride and then drying and concentrating the extract in vacuo, there was obtained an oil which eventually crystallised. The resulting crude product used immediately.
Workup
- concentrationIt was concentrated almost to dryness
- additionthe added to water
- extractionAfter extraction with methylene chloride
- customdrying
- concentrationconcentrating the
- extractionextract in vacuo
- customthere was obtained an oil which
- customeventually crystallised
Sources & evidence
- ORD record
- ord-beebd25ad6274fa18fe8c1bdf83185db
- Source dataset
- uspto-grants-1991_01
- Patent number
- US04983755
Reaction notes
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