Reaktionsgleichung
[F:1][C:2]1[CH:7]=[CH:6][C:5]([N:8]2[CH2:13][CH2:12][NH:11][CH2:10][CH2:9]2)=[CH:4][CH:3]=1.[O:14]=[C:15]1[C:19]([C:26]2[CH:31]=[CH:30][CH:29]=[CH:28][CH:27]=2)([C:20]2[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=2)[CH2:18][CH2:17][N:16]1[CH2:32][C:33](O)=[O:34].Cl.C(N=C=NCCCN(C)C)C>ClCCl>[F:1][C:2]1[CH:3]=[CH:4][C:5]([N:8]2[CH2:13][CH2:12][N:11]([C:33](=[O:34])[CH2:32][N:16]3[CH2:17][CH2:18][C:19]([C:20]4[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=4)([C:26]4[CH:31]=[CH:30][CH:29]=[CH:28][CH:27]=4)[C:15]3=[O:14])[CH2:10][CH2:9]2)=[CH:6][CH:7]=1Komponenten
Edukt 3
Produkt 1
Reagenzien, Katalysatoren, Lösungsmittel 1
Versuchsvorschrift
A solution of 1-(4-fluorophenyl)piperazine (0.034 g, 0.186 mmol), 2-(2-oxo-3,3-diphenylpyrrolidin-1-yl)acetic acid (Example 1C, 0.050 g, 0.169 mmol) and N1-((ethylimino)methylene)-N3,N3-dimethylpropane-1,3-diamine hydrochloride (0.049 g, 0.254 mmol) in dichloromethane (2 mL) was stirred at room temperature. After stirring overnight, the reaction mixture was loaded directly onto a SF15-12 silica gel column (Analogix®, Burlington, Wis.), and the title compound was eluted using a gradient of 5% to 75% ethyl acetate/hexanes over 25 minutes (flow=30 mL/minute). 1H NMR (300 MHz, CDCl3) δ ppm 7.27-7.38 (m, 8H), 7.18-7.25 (m, 2H), 6.94-7.01 (m, 2H), 6.80-6.85 (m, 2H), 4.24 (s, 2H), 3.73 (t, J=4.9 Hz, 2H), 3.54-3.60 (m, 2H), 3.54 (t, J=6.5 Hz, 2H), 3.02 (t, J=5.0 Hz, 2H), 2.89 (t, J=5.2 Hz, 2H), 2.82 (t, J=6.5 Hz, 2H).
Aufarbeitung
- washthe title compound was eluted
- customover 25 minutes
Quellen und Nachweise
- ORD-Eintrag
- ord-0726667cc4fa4343a0972430e5fd662d
- Quelldatensatz
- uspto-grants-2011_10
- Patentnummer
- US08044069B2
Verknüpfte Notizen
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