反应详情

温度

170 °C

A mixture of (R)-4-(5-chloro-2,3-dihydro-furo[2,3-c]pyridin-2-yl)-piperidine-1-carboxylic acid tert-butyl ester (0.40 g), 1-methanesulfonyl-4-(4,4,5,5-tetramethyl-[1,3,2]dioxaborolan-2-yl)-1,2,3,6-tetrahydro-pyridine (0.38 g), 2 M aqueous Na2CO3 solution (1.3 mL), and 1,4-dioxane (8 mL) is sparged with argon for 5 min. Tetrakis(triphenylphosphine)palladium(0) (0.10 g) is added and the mixture is stirred in a microwave oven at 170° C. for 1 h. After cooling to room temperature, water is added and the resulting mixture is extracted with ethyl acetate. The combined extract is washed with brine, dried (Na2SO4), and concentrated. The residue is chromatographed on silica gel (cyclohexane/ethyl acetate 3:7→0:1) to give the title compound. Mass spectrum (ESI+): m/z=464 [M+H]+.

1. customis sparged with argon for 5 min
2. additionTetrakis(triphenylphosphine)palladium(0) (0.10 g) is added
3. temperatureAfter cooling to room temperature
4. additionwater is added
5. extractionthe resulting mixture is extracted with ethyl acetate
6. extractionThe combined extract
7. washis washed with brine
8. dry with materialdried (Na2SO4)
9. concentrationconcentrated
10. customThe residue is chromatographed on silica gel (cyclohexane/ethyl acetate 3:7→0:1)