N'-(6-chloro-3-pyridazinyl)-2,2-dimethylpropionohydrazide → 3-Tert-butyl-6-chloro-(1,2,4)triazolo(4,3-b)pyridazine
Reaction equation
[Cl:1][C:2]1[N:7]=[N:6][C:5]([NH:8][NH:9][C:10](=O)[C:11]([CH3:14])([CH3:13])[CH3:12])=[CH:4][CH:3]=1>C(OCC)(=O)C>[C:11]([C:10]1[N:6]2[N:7]=[C:2]([Cl:1])[CH:3]=[CH:4][C:5]2=[N:8][N:9]=1)([CH3:14])([CH3:13])[CH3:12]Participants
3
Reactant 1
Product 1
Reagents, catalysts & solvents 1
Conditions
- Temperature
- 170 °C
Procedure
2.78 g of N′-(6-chloro-3-pyridazinyl)-2,2-dimethylpropionohydrazide was stirred under heating at an external temperature of 170° C. for 10 minutes. After cooling, the reaction mixture was dissolved in ethyl acetate, subjected to silica gel column chromatography, and eluted with ethyl acetate. The desired fraction was collected and concentrated under reduced pressure; the precipitated crystal was washed with hexane and dried to yield 2.38 g of the title compound.
Workup
- temperatureAfter cooling
- washeluted with ethyl acetate
- customThe desired fraction was collected
- concentrationconcentrated under reduced pressure
- washthe precipitated crystal was washed with hexane
- customdried
Sources & evidence
- ORD record
- ord-6939f07204c84e54b0a440a2ab5134a7
- Source dataset
- uspto-grants-2003_08
- Patent number
- US06610694B1
Reaction notes
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