Reaktion #2028937

Reaktionsgleichung

Xantphos

2,2′-dichloro-[4,4′]-bipyridinyl

2-amino-1-methoxypropane

sodium tert-butoxide

→

(2′-Chloro-[4,4′]bipyridinyl-2-yl)-(2-methoxy-1-methyl-ethyl)-amine

Lösungsmittel

toluene

Reaktionsbedingungen

Aufarbeitung

1. 1
   workup.STIRRINGThe mixture stirred at 60° C. for 6 hours
2. 2
   workup.ADDITIONpoured onto water
3. 3
   Extraktionextracted with ethyl acetate
4. 4
   Trocknendried over Na2SO4
5. 5
   Einengenconcentrated under reduced pressure
6. 6
   SonstigeThe residue was purified

Vorschrift

Xantphos (32 mg), and Pd2(dba)3 (25 mg) were suspended in toluene (8 ml) and stirred under argon for 10 mins, then 2,2′-dichloro-[4,4′]-bipyridinyl (250 mg), 2-amino-1-methoxypropane (0.117 ml) and sodium tert-butoxide (150 mg) were added. The mixture stirred at 60° C. for 6 hours then cooled to room temp, poured onto water and extracted with ethyl acetate, dried over Na2SO4 and concentrated under reduced pressure. The residue was purified by passing the crude mixture down Kieselgel using a gradient of hexane and ethyl acetate as the eluent.

Quelle