Flumexadol → HCID 118323819, Verbindung
Reaktionsgleichung
[F:1][C:2]([F:16])([F:15])[C:3]1[CH:4]=[C:5]([CH:9]2[O:14][CH2:13][CH2:12][NH:11][CH2:10]2)[CH:6]=[CH:7][CH:8]=1.[F:17][C:18]([F:26])([F:25])[C:19](=[CH2:24])[C:20]([O:22][CH3:23])=[O:21]>>[F:17][C:18]([F:26])([F:25])[CH:19]([CH2:24][N:11]1[CH2:12][CH2:13][O:14][CH:9]([C:5]2[CH:6]=[CH:7][CH:8]=[C:3]([C:2]([F:1])([F:15])[F:16])[CH:4]=2)[CH2:10]1)[C:20]([O:22][CH3:23])=[O:21]Komponenten
3
Versuchsvorschrift
In a 5 mL round-bottomed flask, 2-(3-(trifluoromethyl)phenyl)morpholine (650 mg, 2.81 mmol) was combined with methyl 2-(trifluoromethyl)acrylate (650 mg, 4.22 mmol; added slowly) to give a colorless solution and stirred at room temperature for 50 min. The crude reaction mixture was concentrated in vacuo to give an oil. The crude material was purified by flash chromatography (silica gel, 40+S, 0% to 30% ethyl acetate in hexanes) to afford 850 mg (78%)(methyl 3,3,3-trifluoro-2-((2-(3-(trifluoromethyl)phenyl)morpholino)-methyl)propanoate as a clear liquid. MH+=386.
Aufarbeitung
- additionadded slowly)
- customto give a colorless solution
- customThe crude reaction mixture
- concentrationwas concentrated in vacuo
- customto give an oil
- customThe crude material was purified by flash chromatography (silica gel, 40+S, 0% to 30% ethyl acetate in hexanes)
Quellen und Nachweise
- ORD-Eintrag
- ord-2bef9af9fcde4139945c44cbef9bcdcf
- Quelldatensatz
- uspto-grants-2016_07
- Patentnummer
- US09388172B2
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