Sodium Phosphate, Dibasic → 1-Methyl-5-(methylthio)-1H-pyrazol-3-amine
Reaction equation
[NH2:1][C:2]1[C:6](C#N)=[C:5]([S:9][CH3:10])[N:4]([CH3:11])[N:3]=1.P([O-])([O-])(O)=O.[Na+].[Na+]>[OH-].[Na+]>[NH2:1][C:2]1[CH:6]=[C:5]([S:9][CH3:10])[N:4]([CH3:11])[N:3]=1Participants
4
Reactant 2
Product 1
Reagents, catalysts & solvents 1
Conditions
- Temperature
- 50 °C
Procedure
5.55 g (33.0 mmol) 3-amino-4-cyano-1-methyl-5-methylmercaptopyrazole heated with 50 ml 32% caustic soda at boiling for 24 hours. The reaction mixture was cooled, made slightly acidic with aqueous sodium hydrogen phosphate, heated for 8 hours at 50° C. and extracted with ethyl acetate. The organic phase was dried over sodium sulfate, concentrated and the residue purified by silica gel chromatography (hexane/ethyl acetate 1:1).
Workup
- temperatureThe reaction mixture was cooled
- extractionextracted with ethyl acetate
- dry with materialThe organic phase was dried over sodium sulfate
- concentrationconcentrated
- customthe residue purified by silica gel chromatography (hexane/ethyl acetate 1:1)
Sources & evidence
- ORD record
- ord-c1a7f84277e14cdcbba2764d7cd70a90
- Source dataset
- uspto-grants-1999_02
- Patent number
- US05869686
Reaction notes
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