Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|
| Edukt | Water | HCID 962 | — |
| Edukt | Triethylamine | HCID 8471 | — |
| Edukt | 3-(Trifluoromethyl)benzoyl chloride | HCID 75257 | — |
| Edukt | Methylamine tetrahydrofuran | HCID 66615946 | — |
| Lösungsmittel | Dichloromethane | HCID 6344 | — |
| Produkt | N-Methyl-3-(trifluoromethyl)benzamide | HCID 1490147 | — |
Reaktionsschritte
A 2M methylamine-THF solution (20 ml) was added to a solution of triethylamine (7 ml) in dichloromethane (70 ml), a solution of 3-(trifluoromethyl)benzoyl chloride (5.0 g) in dichloromethane (30 ml) was added dropwise thereto under ice cooling, followed by stirring at room temperature for 72 hours. The reaction solution was poured into water, followed by extraction with chloroform. The organic layer was washed with saturated aqueous sodium bicarbonate solution and then saturated brine in this order and dried over anhydrous magnesium sulfate, and the solvent was then evaporated under reduced pressure. The residue was dissolved again in ethyl acetate, washed with saturated aqueous sodium bicarbonate solution and then saturated brine in this order, and dried over anhydrous magnesium sulfate, and the solvent was evaporated under reduced pressure. The resulting solid was washed with diisopropylether, to obtain, as a colorless solid, N-methyl-3-(trifluoromethyl)benzamide (1.34 g).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patentnummer | US08377923B2 |
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| Quelldatensatz | uspto-grants-2013_02 |
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| ORD ID | ord-74200f13a85849c9a1e20e868422464d |
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| Quellennotiz | uspto-grants-2013_02 |
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