1-Methylpiperazine → Piperazine, 1-[2-bromo-5-(trifluoromethyl)phenyl]-4-methyl-
Reaktionsgleichung
[CH3:1][N:2]1[CH2:7][CH2:6][NH:5][CH2:4][CH2:3]1.[Br:8][C:9]1[CH:14]=[CH:13][C:12]([C:15]([F:18])([F:17])[F:16])=[CH:11][C:10]=1F>>[Br:8][C:9]1[CH:14]=[CH:13][C:12]([C:15]([F:18])([F:17])[F:16])=[CH:11][C:10]=1[N:5]1[CH2:6][CH2:7][N:2]([CH3:1])[CH2:3][CH2:4]1Komponenten
3
Reaktionsbedingungen
- Temperatur
- 180 °C
Versuchsvorschrift
A microwave vial was charged with 1-methylpiperazine (1.371 mL, 12.35 mmol) and 4-bromo-3-fluorobenzotrifluoride (1.000 mL, 4.12 mmol), and was heated under microwave irradiation at 180° C. for 90 minutes. The reaction was concentrated under a vacuum, and the solids were then filtered and washed with DCM (solids contained only minor amounts of product). The filtrate was then concentrated under a vacuum to yield 1-(2-bromo-5-(trifluoromethyl)phenyl)-4-methylpiperazine, mixed with starting bromide. Material was used without further purification.
Aufarbeitung
- concentrationThe reaction was concentrated under a vacuum
- filtrationthe solids were then filtered
- washwashed with DCM (solids
- concentrationThe filtrate was then concentrated under a vacuum
Quellen und Nachweise
- ORD-Eintrag
- ord-548a6f0e50b34849b0bd622e210c18aa
- Quelldatensatz
- uspto-grants-2016_05
- Patentnummer
- US09346798B2
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