Reaktionsgleichung
Cl.[Br:2][C:3]1[CH:8]=[CH:7][C:6]([N:9]2[CH2:14][CH2:13][NH:12][CH2:11][CH2:10]2)=[CH:5][CH:4]=1.[C:15]([O:19][C:20](=[O:30])[CH:21]([CH2:25][S:26](Cl)(=[O:28])=[O:27])[CH:22]([CH3:24])[CH3:23])([CH3:18])([CH3:17])[CH3:16].C(N(CC)CC)C>ClCCl>[C:15]([O:19][C:20](=[O:30])[CH:21]([CH2:25][S:26]([N:12]1[CH2:13][CH2:14][N:9]([C:6]2[CH:5]=[CH:4][C:3]([Br:2])=[CH:8][CH:7]=2)[CH2:10][CH2:11]1)(=[O:27])=[O:28])[CH:22]([CH3:24])[CH3:23])([CH3:17])([CH3:18])[CH3:16]Komponenten
5
Edukt 3
Produkt 1
Reagenzien, Katalysatoren, Lösungsmittel 1
Versuchsvorschrift
A stirred suspension of 4-bromophenylpiperazine hydrochloride (2.84 g) and 2-chlorosulfonylmethyl-3-methyl-butyric acid tert-butyl ester (2.77 g) [preparation described in WO-A-98/05635] in dichloromethane (50 ml), cooled in an ice-bath, was treated with triethylamine (2 99 ml). The reaction was then stirred at room temperature for 2 h. The reaction mixture was then evaporated in vacuo, and the residue was dissolved in ethyl acetate (75 ml) and washed with 1% aqueous citric acid (2×50 ml), water (50 ml), saturated sodium bicarbonate (50 ml), saturated brine (50 ml), dried (MgSO4) and concentrated in vacuo to provide the title compound as a pale yellow gum (3.81 g, 79%).
Aufarbeitung
- custompreparation
- temperaturecooled in an ice-bath
- customThe reaction mixture was then evaporated in vacuo
- dissolutionthe residue was dissolved in ethyl acetate (75 ml)
- washwashed with 1% aqueous citric acid (2×50 ml), water (50 ml), saturated sodium bicarbonate (50 ml), saturated brine (50 ml)
- dry with materialdried (MgSO4)
- concentrationconcentrated in vacuo
Quellen und Nachweise
- ORD-Eintrag
- ord-a8811c805f3a4f718c2c27961760b7a6
- Quelldatensatz
- uspto-grants-2004_10
- Patentnummer
- US06809100B2
Verknüpfte Notizen
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