Diiodomethane → HCID 18326232, Verbindung
Reaktionsgleichung
N(OCCC(C)C)=O.N[C:10]1[C:11]([Cl:26])=[CH:12][C:13]([F:25])=[C:14]([C:16]2[C:20]([CH3:21])=[C:19]([C:22]#[N:23])[N:18]([CH3:24])[N:17]=2)[CH:15]=1.[I:27]CI>>[Cl:26][C:11]1[C:10]([I:27])=[CH:15][C:14]([C:16]2[C:20]([CH3:21])=[C:19]([C:22]#[N:23])[N:18]([CH3:24])[N:17]=2)=[C:13]([F:25])[CH:12]=1Komponenten
4
Reaktionsbedingungen
- Temperatur
- 22 °C
Versuchsvorschrift
5.86 g of isoamyl nitrite are added dropwise at a temperature of below 15° C. to a solution of 2.64 g of 3-(5-amino-4-chloro-2-fluoro-phenyl)-4-methyl-5-cyano-1-methyl-[1H]-pyrazole in 54 g (16 ml) of diiodomethane. The reaction mixture is stirred for 14 hours at 22° C., and excess diiodomethane is evaporated in vacuo. All the diiodomethane is subsequently distilled off at 70-75° C./14 torr, and the crude product is purified over a silica gel column (eluent: ethyl acetate/hexane 1/5). The desired product is obtained in a yield of 1.88 g (50.2% of theory).