反应详情

温度

20 °C

To a solution of 2-(methyloxy)-5-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)-3-pyridinamine (0.5 g, 1.999 mmol) in pyridine (5 ml) was added methanesulphonyl chloride (0.309 ml, 4.00 mmol) and the mixture stirred at 20° C. for 18 hr when the solvent was removed in vacuo. The residue was partitioned between saturated sodium bicarbonate solution (10 ml) and dichloromethane (20 ml), separated by hydrophobic frit and purified by silica (70 g) cartridge on Flashmaster II using a gradient of dichloromethane and methanol to give the title compound as a brown solid (0.46 g).

1. customwas removed in vacuo
2. customThe residue was partitioned between saturated sodium bicarbonate solution (10 ml) and dichloromethane (20 ml)
3. customseparated by hydrophobic frit
4. custompurified by silica (70 g) cartridge on Flashmaster II