反応 #2028938

反応方程式

BINAP

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

3-chloroaniline

potassium carbonate

→

N*2′*-(3-Chloro-phenyl)-N*2*-(2-methoxy-1-methyl-ethyl)-[4,4′]bipyridinyl-2,2′-diamine

溶媒

toluene

反応条件

後処理

1. 1
   workup.STIRRINGThe mixture was stirred at 110° C. for 5 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

Pd(OAc)2 (8 mg) and BINAP (16 mg) were suspended in toluene (10 ml) and stirred under argon for 10 mins, then (2′-Chloro-[4,4′]bipyridinyl-2-yl)-(2-methoxy-1-methyl-ethyl)-amine (90 mg), 3-chloroaniline (124 mg) and potassium carbonate (890 mg) were added. The mixture was stirred at 110° C. for 5 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 1:99 THF:CH2Cl2 as the eluent.

出典