反应详情

Tris(dibenzylideneacetone)dipalladium (23 mg; 0.03 mmol), 2,2′-bis(diphenylphosphino)-1,1′-binaphthyl (46 mg; 0.07 mmol), sodium tert-butoxide (176 mg; 1.83 mmol), 1-bromo-4-trifluoromethylsulfanyl-benzene (314 mg; 1.22 mmol) and 4-amino-piperidine-1-carboxylic acid tert-butyl ester (302 mg; 1.51 mmol) are suspended in dry toluene (5 mL) and the mixture is irradiated in a mono-mode microwave oven for 20 minutes at 120° C. The mixture is then cooled down to room temperature, is diluted with ethyl acetate (15 mL), filtered and concentrated under reduced pressure. The crude residue is then diluted in dichloromethane (15 mL) and filtered over a short silica gel pad. The desired product is eluted from the silica gel pad with dichloromethane and the fractions of interest are concentred under reduced pressure to afford the desired product (220 mg; 0.59 mmol).

1. customthe mixture is irradiated in a mono-mode microwave oven for 20 minutes at 120° C
2. filtrationfiltered
3. concentrationconcentrated under reduced pressure
4. additionThe crude residue is then diluted in dichloromethane (15 mL)
5. filtrationfiltered over a short silica gel pad
6. washThe desired product is eluted from the silica gel pad with dichloromethane