Reaktion #165205
ord-19a4adf46e3a41f896089fe4a5947ea1
Reaktionsgleichung
Reagenzien
Keine
Lösungsmittel
Reaktionsbedingungen
Temperatur
100°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.
Aufarbeitung
- 1TemperaturThis mixture was cooled to room temperature
- 2Einengenconcentrated under a reduced pressure
- 3workup.ADDITIONdiluted with ethyl acetate
- 4WaschenThe organic layer was washed with saturated aqueous sodium chloride
- 5Trocknendried over anhydrous magnesium sulfate
- 6Filtrationfiltered
- 7EinengenThe filtrate was concentrated under a reduced pressure
Vorschrift
A mixture of 4-cyclohexyloxy-benzaldehyde (2.84 g, 13.9 mmol) described in Manufacturing Example 79-1-1, nitromethane (3.74 mL, 69.5 mmol), ammonium acetate (2.14 g, 27.8 mmol) and acetic acid (30 mL) was stirred for 14 hours at 100° C. This mixture was cooled to room temperature, concentrated under a reduced pressure, and diluted with ethyl acetate. The organic layer was washed with saturated aqueous sodium chloride, dried over anhydrous magnesium sulfate, and filtered. The filtrate was concentrated under a reduced pressure to obtain the title compound (3.3 g).