反应详情

1 g of 4-[4-methoxy-5-(2-methoxy-phenoxy)-6-(5-methyl-pyridine-2-sulfonylamino)-pyrimidin-2-yl]-pyridine-2-carboxylic acid amide, product of example 20, dissolved in a mixture of THF/dioxane (40 ml/30 ml) were treated at RT with 3N HCl (40 ml) and the solution was refluxed for 24 h, further THF (12 ml) and 3M HCl (12 ml) was then added and the solution was heated to reflux for further 24 h until the transformation was complete according to TLC analysis. The reaction mixture was concentrated in vacuo and the product was extracted into CH2Cl2. The organic layer was dried over Na2SO4, the solvent removed in vacuo. The remaining crystalline solid was washed with ether and dried in a vacuum to give 4-[4-methoxy-5-(2-methoxy-phenoxy)-6-(5-methyl-pyridine-2-sulfonylamino)-pyrimidin-2-yl]-pyridine-2-carboxylic acid as an off-white solid. ISN mass spectrum, m/e 522 (M−1 calculated for C24H21N5O7S: 522).

1. temperaturethe solution was refluxed for 24 h
2. temperaturethe solution was heated
3. temperatureto reflux for further 24 h until the transformation
4. concentrationThe reaction mixture was concentrated in vacuo
5. extractionthe product was extracted into CH2Cl2
6. dry with materialThe organic layer was dried over Na2SO4
7. customthe solvent removed in vacuo
8. washThe remaining crystalline solid was washed with ether
9. customdried in a vacuum