反应详情

2 M aqueous Na2CO3 solution (0.30 mL) is added to a mixture of 5-chloro-1″-tert-butoxycarbonyl-dispiro[2,3-dihydrofuro[2,3-c]pyridine-2,1′-cyclobutane-3′,4″-piperidine] (0.10 g), 4-(methanesulfonyl)phenylboronic acid (0.08 g), 1,4-dioxane (1.5 mL), and methanol (0.5 mL) at room temperature. The mixture is sparged with Ar for 10 min prior to addition of PdCl2[1,1′-bis(diphenylphosphino)-ferrocene]*CH2Cl2 complex (20 mg). The resulting mixture is heated to reflux temperature and stirred at this temperature for 2 h. After cooling to room temperature, water and methanol are added and the resulting mixture is filtered. The filtrate is concentrated and the residue is chromatographed on reversed phase (HPLC, methanol/water) to give the title compound. LC (method 2): tR=1.72 min; Mass spectrum (ESI+): m/z=485 [M+H]+.

1. customThe mixture is sparged with Ar for 10 min
2. additionto addition of PdCl2[1,1′-bis(diphenylphosphino)-ferrocene]*CH2Cl2 complex (20 mg)
3. temperatureThe resulting mixture is heated
4. temperatureto reflux temperature
5. additionwater and methanol are added
6. filtrationthe resulting mixture is filtered
7. concentrationThe filtrate is concentrated
8. customthe residue is chromatographed on reversed phase (HPLC, methanol/water)