Reaktion #165205

ord-19a4adf46e3a41f896089fe4a5947ea1

Lösungsmittel

Reaktionsbedingungen

Temperatur
100°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    TemperaturThis mixture was cooled to room temperature
  2. 2
    Einengenconcentrated under a reduced pressure
  3. 3
    workup.ADDITIONdiluted with ethyl acetate
  4. 4
    WaschenThe organic layer was washed with saturated aqueous sodium chloride
  5. 5
    Trocknendried over anhydrous magnesium sulfate
  6. 6
    Filtrationfiltered
  7. 7
    EinengenThe 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).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08841327B2uspto-grants-2014_09