反应详情

温度

100 °C

To a solution of 700 mg (2.6 mmol) 2-chloro-4-methyl-6-morpholino-pyridine-3-carboxylic acid methylester and 1.39 g (3.9 mmol) tributyl(3-methoxyprop-1-ynyl)stannane in dioxane (10 ml) was added 273 mg (0.39 mmol) PdCl2(PPh3)2. Then the reaction solution was heated at 100° C. for 16 h. After cooling to RT the mixture was filtered through celite and the filtrate was concentrated in vacuo. The residue was dissolved in EtOAc and washed with water. The organic layer was dried over Na2SO4 and concentrated in vacuo. Purification of the residue by CC (5% KF-silica, hexane/EtOAc 19:1) provided 500 mg (1.64 mmol, 63%) 2-(3-methoxyprop-1-ynyl)-4-methyl-6-morpholino-pyridine-3-carboxylic acid methylester.

1. temperatureAfter cooling to RT the mixture
2. filtrationwas filtered through celite
3. concentrationthe filtrate was concentrated in vacuo
4. dissolutionThe residue was dissolved in EtOAc
5. washwashed with water
6. dry with materialThe organic layer was dried over Na2SO4
7. concentrationconcentrated in vacuo
8. customPurification of the residue by CC (5% KF-silica, hexane/EtOAc 19:1)