Hydrochloric Acid → 2-(Fluoro-dichloro-methyl)-8-methyl-4-chloro-quinoline

HRID 542931

Reaktionsgleichung

Reaktionsgleichung von HRID 542931
[Cl:1][C:2]([Cl:16])(Cl)[C:3]1[CH:12]=[C:11]([Cl:13])[C:10]2[C:5](=[C:6]([CH3:14])[CH:7]=[CH:8][CH:9]=2)[N:4]=1.[Sb](Cl)(Cl)(Cl)(Cl)Cl.[Sb](F)(F)(F)(F)[F:24].Cl>ClCCl>[F:24][C:2]([Cl:16])([Cl:1])[C:3]1[CH:12]=[C:11]([Cl:13])[C:10]2[C:5](=[C:6]([CH3:14])[CH:7]=[CH:8][CH:9]=2)[N:4]=1

Komponenten

6

Edukt 4

HCID 313Hydrochloric AcidHCID 24294Antimony pentachlorideHCID 24557Antimony pentafluorideHCID 156222554-Chloro-8-methyl-2-(trichloromethyl)quinoline

Produkt 1

HCID 156222562-(Fluoro-dichloro-methyl)-8-methyl-4-chloro-quinoline

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344DichloromethaneLösungsmittel

Versuchsvorschrift

3.0 g of 2-trichloromethyl-8-methyl-4-chloro-quinoline are dissolved in 45 ml of dry dichloromethane and under intense stirring 1.5 ml of antimony-penta-chloride and 1.0 ml of antimony-penta-fluoride are added by dropping at a temperature of -5° to 0° C. The mixture is stirred at this temperature for 4 hours and allowed to stand at room temperature for 48 hours. 6 ml of icy concentrated hydrochloric acid are added, the precipitate is filtered, washed with some dichloromethane, the filtrate is separated, dried, filtered and evaporated. 2.1 g solid product are obtained which is recrystallized from heptane: 1.9 g of a yellowish crystalline substance, 68.2%, m.p.: 90°-94° C.

Aufarbeitung

  1. additionare added
  2. customby dropping at a temperature of -5° to 0° C
  3. waitto stand at room temperature for 48 hours
  4. filtrationthe precipitate is filtered
  5. washwashed with some dichloromethane
  6. customthe filtrate is separated
  7. customdried
  8. filtrationfiltered
  9. customevaporated

Quellen und Nachweise

ORD-Eintrag
ord-f9a3a7745e0a4edeb479b8851e6d1311
Quelldatensatz
uspto-grants-1987_04
Patentnummer
US04659834

Verknüpfte Notizen

Wird geladen…