反応 #2028937

反応方程式

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

溶媒

toluene

反応条件

後処理

1. 1
   workup.STIRRINGThe mixture stirred at 60° C. for 6 hours
2. 2
   workup.ADDITIONpoured onto water
3. 3
   抽出extracted with ethyl acetate
4. 4
   乾燥dried over Na2SO4
5. 5
   濃縮concentrated under reduced pressure
6. 6
   その他The residue was purified

実験手順

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.

出典