Nitromethane → HCID 63051539, compound
Reaction equation
C([O-])(=O)C.[NH4+].[F:6][C:7]1[CH:8]=[C:9]([CH:12]=[C:13]([F:16])[C:14]=1[F:15])[CH:10]=O.[N+:17]([CH3:20])([O-:19])=[O:18]>C(O)(=O)C>[F:6][C:7]1[CH:8]=[C:9](/[CH:10]=[CH:20]/[N+:17]([O-:19])=[O:18])[CH:12]=[C:13]([F:16])[C:14]=1[F:15]Participants
5
Reactant 3
Product 1
Reagents, catalysts & solvents 1
Conditions
- Temperature
- 100 °C
Procedure
Ammonium acetate (7.3 g) was added to a solution of 3,4,5-trifluorobenzaldehyde (12.6 g) and nitromethane (17.1 mL) in acetic acid (50 mL), and the reaction solution was stirred at 100° C. for three hours. The reaction solution was left to cool to room temperature and then concentrated under reduced pressure. Ethyl acetate and saturated sodium bicarbonate water were added to the residue, and the organic layer was separated. The resulting organic layer was dried over anhydrous magnesium sulfate and then concentrated under reduced pressure. The residue was purified by silica gel column chromatography (heptane->heptane:ethyl acetate=9:1) to obtain 10.5 g of the title compound. The property values of the compound are as follows.
Workup
- waitThe reaction solution was left
- temperatureto cool to room temperature
- concentrationconcentrated under reduced pressure
- additionEthyl acetate and saturated sodium bicarbonate water were added to the residue
- customthe organic layer was separated
- dry with materialThe resulting organic layer was dried over anhydrous magnesium sulfate
- concentrationconcentrated under reduced pressure
- customThe residue was purified by silica gel column chromatography (heptane->heptane:ethyl acetate=9:1)
Sources & evidence
- ORD record
- ord-38806fb729d146c7afe875e3688a8b4c
- Source dataset
- uspto-grants-2011_11
- Patent number
- US08048878B2
Reaction notes
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