反应详情

1.46 g of 5-methyl-pyridine-2-sulfonic acid [2-(3-benzyloxy-phenyl)-6-methoxy-5-(2-methoxy-phenoxy)-pyrimidin-4-yl]-amide were dissolved in dioxane (25 ml) by gentle warming than ethanol (50 ml) was added followed by cyclohexadiene (6 g) and palladium on charcoal, 10%, (1.46 g). The solution was refluxed for 20 h, the catalyst removed by filtration and the solution concentrated on a rotary evaporator. The yellow crystalline solid that precipitated was collected, washed with ether and dried in a vacuum to give the desired 5-methyl-pyridine-2-sulfonic acid [2-(3-hydroxy-phenyl)-6-methoxy-5-(2-methoxy-phenoxy)-pyrimidin-4-yl]-amide as off-white crystals. ISP mass spectrum, m/e 495.2 (M+1 calculated for C24H22N4O6S1: 495). Melting point 211°-216° C.

1. additionwas added
2. temperatureThe solution was refluxed for 20 h
3. customthe catalyst removed by filtration
4. concentrationthe solution concentrated on a rotary evaporator
5. customThe yellow crystalline solid that precipitated
6. customwas collected
7. washwashed with ether
8. customdried in a vacuum