反应详情

温度

45 °C

Benzylsulfamic acid [6-(2-hydroxy-ethoxy)-2-methanesulfonyl-5-(2-methoxy-phenoxy)-pyrimidin-4-yl]-amide (85 mg) were dissolved in THF (2 ml) and morpholine (2 ml) was added. The reaction mixture was stirred at 45° C. for 48 hours, poured onto water, acidified with solid citric acid and extracted with EtOAc (2×). The combined EtOAc layers were washed with 10% citric acid solution and with brine, dried over magnesium sulfate, filtered and the solvent was evaporated. The crude product was purified by chromatography on plates with toluene/EtOAc=1/1 to give benzylsulfamic acid [6-(2-hydroxy-ethoxy)-5-(2-methoxy-phenoxy)-2-morpholin-4-yl-pyrimidin-4-yl]-amide (Example 205) (60 mg). LC-MS: tR=4.69; [M+H]+=532.15.

1. additionpoured onto water
2. extractionextracted with EtOAc (2×)
3. washThe combined EtOAc layers were washed with 10% citric acid solution and with brine
4. dry with materialdried over magnesium sulfate
5. filtrationfiltered
6. customthe solvent was evaporated
7. customThe crude product was purified by chromatography on plates with toluene/EtOAc=1/1