反应详情

温度

85 °C

To a solution of potassium tert.-butoxide (366.5 mg) in ethylene glycol (5 ml) was added 1,2-dimethoxy ethane (5 ml) and ethanesulfonic acid [6-chloro-5-(2-methoxy-phenoxy)-[2,2′]bipyrimidinyl-4-yl]-amide (420 mg). The reaction mixture was heated to 85° C. for 7 days, concentrated in vacuo, poured onto water, acidified by 2N HCl, and extracted with ethyl acetate. The combined organic extracts were dried over magnesium sulfate and concentrated in vacuo. The precipitated product was washed with diethyl ether, filtered and dried at HV to give ethanesulfonic acid [6-(2-hydroxy-ethoxy)-5-(2-methoxy-phenoxy)-[2,2′]bipyrimidinyl-4-yl]-amide (400 mg). LC-MS: tR: 3.45, [M+H]+: 448.24.

1. concentrationconcentrated in vacuo
2. additionpoured onto water
3. extractionextracted with ethyl acetate
4. dry with materialThe combined organic extracts were dried over magnesium sulfate
5. concentrationconcentrated in vacuo
6. washThe precipitated product was washed with diethyl ether
7. filtrationfiltered
8. customdried at HV