反応 #56615

反応方程式

(5R)-1-allyl-5-[4′-(trifluoromethoxy)-1,1′-biphenyl-4-yl]-2-pyrrolidinone

p-toluenesulphonic acid hydrate

THF

H2O

→

(5R)-5-[4′-(Trifluoromethoxy)-1,1′-biphenyl-4-yl]-2-pyrrolidinone

溶媒

NaHCO3

ethyl acetate

反応条件

後処理

1. 1
   workup.ADDITIONare added
2. 2
   温度The yellow suspension is heated
3. 3
   温度under reflux for 3 h
4. 4
   ろ過filtered through kieselguhr
5. 5
   乾燥The combined organic phases are dried (Na2SO4)
6. 6
   濃縮concentrated under reduced pressure

実験手順

Under argon, (5R)-1-allyl-5-[4′-(trifluoromethoxy)-1,1′-biphenyl-4-yl]-2-pyrrolidinone (XVII-1) (0.41 g, 1.14 mmol) is initially charged in a Schlenk tube together with Pd[PPh3]4 (131.7 mg, 0.114 mmol) and p-toluenesulphonic acid hydrate (0.52 g, 2.74 mmol), and THF (2 ml, degassed) and 1 ml of H2O are added. The yellow suspension is heated under reflux for 3 h. For work-up, the mixture, which was cooled to room temperature, is diluted with NaHCO3 solution and admixed with ethyl acetate and filtered through kieselguhr. The combined organic phases are dried (Na2SO4) and concentrated under reduced pressure.

出典