Sodium Hydroxide → 1H-Pyrazol-5-amine, 1-[2,3,6-trichloro-4-(trifluoromethyl)phenyl]-
Reaction equation
Cl[O-].[Na+].[Cl:4][C:5]1[C:10]([Cl:11])=[C:9]([C:12]([F:15])([F:14])[F:13])[CH:8]=[C:7]([Cl:16])[C:6]=1[NH:17][NH:18][CH2:19][CH2:20][C:21]#[N:22].[OH-].[Na+]>C(O)C>[Cl:4][C:5]1[C:10]([Cl:11])=[C:9]([C:12]([F:14])([F:15])[F:13])[CH:8]=[C:7]([Cl:16])[C:6]=1[N:17]1[C:21]([NH2:22])=[CH:20][CH:19]=[N:18]1Participants
5
Reactant 3
Product 1
Reagents, catalysts & solvents 1
Conditions
- Temperature
- 20 °C
Procedure
38 g of sodium hypochlorite solution (prepared by passing about 18 g of chlorine into 220 g of 20% strength sodium hydroxide solution) are added dropwise to 13.5 (0.04 mol) of N-(2,3,6-trichloro-4-trifluoromethylphenyl)-N'-2-cyano-ethylhydrazine in 80 ml of ethanol at 10° C. The mixture is stirred at 20° C. for 16 hours, 0.5 g of solid sodium hydroxide are added and the mixture is subsequently stirred for 6 hours. It is concentrated, the residue is taken up in methylene chloride, the mixture is washed twice with water and concentrated and the residue is distilled. 10 g (76% of theory) of 1-(2,3,6-trichloro-4-trifluoromethylphenyl)-5-amino-pyrazole are obtained.
Workup
- stirringthe mixture is subsequently stirred for 6 hours
- concentrationIt is concentrated
- washthe mixture is washed twice with water
- concentrationconcentrated
- distillationthe residue is distilled
Sources & evidence
- ORD record
- ord-ea496273e1094722a61010bd6d719ab8
- Source dataset
- uspto-grants-1989_04
- Patent number
- US04824960
Reaction notes
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