Reaktion #167716

Reaktionsgleichung

2-Chloro-3-fluorobenzaldehyde

(R)-(+)-2-methyl-2-propanesulfinamide

→

N-[1-(2-Chloro-3-fluorophenyl)meth-(E)-ylidene]-2-methylpropane-2-sulfinamide

Lösungsmittel

dichloromethane

Reaktionsbedingungen

Aufarbeitung

1. 1
   TemperaturThe mixture was heated for three hours
2. 2
   Temperaturunder reflux
3. 3
   workup.ADDITIONpoured onto ice (150 g)
4. 4
   FiltrationThe mixture was filtered through kieselguhr
5. 5
   Extraktionthe filtrate was extracted with dichloromethane (3×50 ml)
6. 6
   TrocknenThe organic phase was dried (Na2SO4)
7. 7
   Filtrationfiltered
8. 8
   Einengenconcentrated under reduced pressure
9. 9
   SonstigeThe product (4 g) was used further without further purification

Vorschrift

2-Chloro-3-fluorobenzaldehyde (2.5 g) and (R)-(+)-2-methyl-2-propanesulfinamide were dissolved in dichloromethane (50 ml), and then titanium(IV) isopropoxide (23.6 ml) was added. The mixture was heated for three hours under reflux, then poured onto ice (150 g) and stirred vigorously for ten minutes. The mixture was filtered through kieselguhr and the filtrate was extracted with dichloromethane (3×50 ml). The organic phase was dried (Na2SO4), filtered and concentrated under reduced pressure. The product (4 g) was used further without further purification.

Quelle