1-Propanol → (3,5,6-Trifluoro-2-pyridyl)hydrazine
Reaction equation
[F:1][C:2]1[C:7]([F:8])=[CH:6][C:5]([F:9])=[C:4](F)[N:3]=1.O.[NH2:12][NH2:13].C(O)CC>ClC>[F:1][C:2]1[C:7]([F:8])=[CH:6][C:5]([F:9])=[C:4]([NH:12][NH2:13])[N:3]=1Participants
5
Reactant 3
Product 1
Reagents, catalysts & solvents 1
Conditions
- Temperature
- 80 °C
Procedure
23.2 g of the compound obtained in Step 1 and 37.3 ml of hydrazine monohydrate were added to 100 ml of n-propanol, and the resulting mixture was heated to 80° C. for 2 hours. The reaction mixture was distilled under a reduced pressure to remove the solvent. The residue thus obtained was dissolved in 100 ml of chloromethane, washed with water, and dried over anhydrous magnesium sulfate. The dried organic layer was concentrated under a reduced pressure to obtain 21.9 g (yield: 83.8%) of the title compound as a light yellow solid.
Workup
- distillationThe reaction mixture was distilled under a reduced pressure
- customto remove the solvent
- customThe residue thus obtained
- washwashed with water
- dry with materialdried over anhydrous magnesium sulfate
- concentrationThe dried organic layer was concentrated under a reduced pressure
Sources & evidence
- ORD record
- ord-10643c8201fd4ce6a458cad26198adc2
- Source dataset
- uspto-grants-2007_05
- Patent number
- US07220863B2
Reaction notes
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