反应详情

温度

50 °C

A mixture of 1.80 g (6.87 mmol) of (5-iodopyridin-2-yl)isopropylamine, 1.40 mL (10.7 mmol) of prop-2-en-1-ol, 1.39 g (16.49 mmol) of sodium hydrogen carbonate, 1.72 g (6.18 mmol) of tetrabutylammonium chloride, and 46 mg (0.20 mmol) of palladium (II) acetate in 10 mL of DMF was stirred under argon for 20 hours at 50° C. The reaction mixture was diluted with water and EtOAc, the organic phase was separated off, washed several times with water, and dried over magnesium sulfate. After the desiccant and solvent had been eliminated, the residue was purified by chromatography (silica gel, PE/EtOAc 1:1). Yield: 300 mg (23% of theoretical); ClIH16N2O (M=192.258); calc.: molpeak (M+H)+:193; found: molpeak (M+H)+:193; HPLC-MS: 3.58 minutes (method G).

1. customthe organic phase was separated off
2. washwashed several times with water
3. dry with materialdried over magnesium sulfate
4. customthe residue was purified by chromatography (silica gel, PE/EtOAc 1:1)
5. custom3.58 minutes (method G)