反应详情

温度

110 °C

A mixture of 4-deoxypyridoxine hydrochloride (0.44 g, 2.8 mmol), copper (I) oxide (0.50 g, 3.5 mmol), dimethylglyoxime (0.15 g, 1.3 mmol), 4-iodobenzonitrile (1.08 g, 4.7 mmol), cesium carbonate (5.00 g, 15.3 mmol), and crushed molecular sieves 3° A (0.6 g) in anhydrous DMF (4 mL) were heated at 110° C. for 12 hours. The reaction mixture was evaporated to dryness, and the crude product purified by column chromatography on silica gel using a gradient of dichloromethane:methyl alcohol (1:0 to 9:1) as eluant to give 4-(5-hydroxymethyl-2,4-dimethyl-pyridin-3-yloxy)-benzonitrile (89) (50 mg, 7% yield).

1. customThe reaction mixture was evaporated to dryness
2. customthe crude product purified by column chromatography on silica gel using a gradient of dichloromethane:methyl alcohol (1:0 to 9:1) as eluant