Water → 5-fluoro-1-methyl-3-trifluoromethyl-1H-pyrazole-4-methanol
Reaktionsgleichung
[BH4-].[Na+].[F:3][C:4]1[N:8]([CH3:9])[N:7]=[C:6]([C:10]([F:13])([F:12])[F:11])[C:5]=1[CH:14]=[O:15].O>CO>[F:3][C:4]1[N:8]([CH3:9])[N:7]=[C:6]([C:10]([F:12])([F:11])[F:13])[C:5]=1[CH2:14][OH:15]Komponenten
Reaktionsbedingungen
- Temperatur
- 0 °C
Versuchsvorschrift
To a solution of 3.9 g (102.6 mmoles) of sodium borohydride dissolved in 500 ml of methanol was added, with ice-cooling, a solution of 36.8 g (187.6 mmoles) of 5-fluoro-1-methyl-3-trifluoromethyl-1H-pyrazole-4-carboaldehyde dissolved in 200 ml of methanol. The resulting mixture was stirred at 0° C. for 30 minutes to give rise to a reaction. After confirmation of the completion of the reaction, the reaction mixture was poured into water, followed by extraction with ethyl acetate. The resulting organic layer was washed with water and an aqueous sodium chloride solution and then dried over anhydrous magnesium sulfate. The resulting solution was subjected to vacuum distillation to remove the solvent contained therein, to obtain 35.4 g (yield: 95.4%) of (5-fluoro-1-methyl-3-trifluoromethyl-1H-pyrazol-4-yl)-methanol.
Aufarbeitung
- additionwas added, with ice-
- temperaturecooling
- customto give rise
- customto a reaction
- customAfter confirmation of the completion of the reaction
- extractionfollowed by extraction with ethyl acetate
- washThe resulting organic layer was washed with water
- dry with materialan aqueous sodium chloride solution and then dried over anhydrous magnesium sulfate
- distillationThe resulting solution was subjected to vacuum distillation
- customto remove the solvent
Quellen und Nachweise
- ORD-Eintrag
- ord-944ba1f887ec40fc8262b0c6de51ec50
- Quelldatensatz
- uspto-grants-2010_11
- Patentnummer
- US07833939B2
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