反应详情

To a mixture of 3-iodo-pyridin-2-ylamine described in Preparation Example 1-1-3 (40.2 g, 183 mmol), trimethylsilyl acetylene (51.7 mL, 366 mmol), copper(I) iodide (3.49 g, 18.3 mmoL), N,N-diisopropyl ethyl amine (63.7 mL, 366 mmol), N-methylpyrrolidinone (200 mL) was added tetrakis(triphenyl phosphine) palladium (0) (10.6 g, 9.15 mmol), which was stirred at room temperature for 3 hours 10 minutes under a nitrogen stream. To the reaction solution was added water and extracted four times with ethyl acetate. The solvent thereof was concentrated under a reduced pressure. The residue was purified by NH silica gel chromatography (heptane:ethyl acetate=4:1). The resulting solution was concentrated under a reduced pressure and the residue was purified by silica gel chromatography (heptane:ethyl acetate=2:1 then 1:1) to obtain the title compound (28.1 g).

1. extractionextracted four times with ethyl acetate
2. concentrationThe solvent thereof was concentrated under a reduced pressure
3. customThe residue was purified by NH silica gel chromatography (heptane:ethyl acetate=4:1)
4. concentrationThe resulting solution was concentrated under a reduced pressure
5. customthe residue was purified by silica gel chromatography (heptane