Methyl iodide → HCID 19990236, compound
Reaction equation
FC(F)(F)[C:3]([NH:5][C:6]1[C:10]([N+:11]([O-:13])=[O:12])=[CH:9][N:8]([CH3:14])[N:7]=1)=O.CI.[OH-].[K+]>CC(C)=O>[CH3:14][N:8]1[CH:9]=[C:10]([N+:11]([O-:13])=[O:12])[C:6]([NH:5][CH3:3])=[N:7]1Participants
5
Reactant 3
Product 1
Reagents, catalysts & solvents 1
Procedure
100 g (4.20 mmoles) of 3-trifluoroacetylamino-1-methyl-4-nitropyrazol are heated with 2.12 g (16.8 mmoles) methyl iodide in 10 ml absolute acetone to 50° C. 940 mg (16.8 mmoles) powdered potassium hydroxide are then added and the reaction mixture is heated to boiling for 5 minutes. The solvent is distilled off in the rotary evaporator in vacuum and the residue is separated by means of column chromatography using silica gel with ether/toluene (5:1).
Workup
- additionare then added
- temperaturethe reaction mixture is heated
- distillationThe solvent is distilled off in the rotary evaporator in vacuum
- customthe residue is separated by means of column chromatography
Sources & evidence
- ORD record
- ord-b5a7cbd289cb4d4c8494d165fb3217cd
- Source dataset
- uspto-grants-1991_10
- Patent number
- US05061289
Reaction notes
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