反应详情

Copper(I) iodide (25 mg) and bis-(triphenylphosphine)-palladium(II)-chloride (30 mg) are added to 6-chloro-4-iodo-pyridin-3-ol (200 mg) in N,N-dimethylformamide (3 mL) under Ar atmosphere at room temperature. Triethylamine (110 μL) is added and the resulting mixture is stirred at room temperature for 1 h. 4-Ethynyl-piperidine-1-carboxylic acid tert-butyl ester (175 mg) dissolved in N,N-dimethylformamide (2 mL) is added dropwise and the mixture is stirred at 55° C. for 3 h. The solvent is evaporated and the residue is chromatographed on silica gel (cyclohexane/ethyl acetate 70:30) to give the title compound. LC (method 2): tR=1.40 min; Mass spectrum (ESI+): m/z=337/339 (Cl) [M+H]+.

1. additionis added dropwise
2. stirringthe mixture is stirred at 55° C. for 3 h
3. customThe solvent is evaporated
4. customthe residue is chromatographed on silica gel (cyclohexane/ethyl acetate 70:30)