Reaktionsgleichung
[Cl:1][C:2]1[C:3]([C:16]#[N:17])=[C:4]([C:8]2[CH:13]=[CH:12][C:11]([Cl:14])=[C:10]([Cl:15])[CH:9]=2)[NH:5][C:6]=1[Cl:7].CC(C)([O-])C.[K+].[CH2:24]([O:26][CH:27](Cl)[CH3:28])[CH3:25]>O1CCCC1>[Cl:1][C:2]1[C:3]([C:16]#[N:17])=[C:4]([C:8]2[CH:13]=[CH:12][C:11]([Cl:14])=[C:10]([Cl:15])[CH:9]=2)[N:5]([CH:24]([O:26][CH2:27][CH3:28])[CH3:25])[C:6]=1[Cl:7]Komponenten
Edukt 3
Produkt 1
Reagenzien, Katalysatoren, Lösungsmittel 1
Versuchsvorschrift
To 4,5-dichloro-2-(3,4-dichlorophenyl)-pyrrole-3-carbonitrile (5.0 g, 0.016 mol) dissolved in 300 mL of tetrahydrofuran is added, portionwise, potassium t-butoxide (2.75 g, 0.025 mol) with ice cooling and stirring. The cooled mixture is treated with a solution of 1-chloroethyl ethyl ether (2.31 g, 0.021 mol) in 15 mL of tetrahydrofuran at 10° C. over a 5 minute period. The mixture is stirred for 1/2 hour at ambient temperatures, evaporated to a volume of 50 mL and poured into a mixture of 200 mL of ethyl acetate and 100 mL of water. The organic layer is separated, washed with water (2×100 mL), saturated NaCl solution (1×100 mL), dried over anhydrous magnesium sulfate and evaporated to give the title product 5.9 g, mp 124°-126° C.
Aufarbeitung
- additionis added
- customevaporated to a volume of 50 mL
- additionpoured into a mixture of 200 mL of ethyl acetate and 100 mL of water
- customThe organic layer is separated
- washwashed with water (2×100 mL), saturated NaCl solution (1×100 mL)
- dry with materialdried over anhydrous magnesium sulfate
- customevaporated
Quellen und Nachweise
- ORD-Eintrag
- ord-112c0cca36bb4ebc9e2e1395a5fe5a64
- Quelldatensatz
- uspto-grants-1997_01
- Patentnummer
- US05591765
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