反应详情

(4-{4-[1-Methyl-1-(methylsulfonyl)ethyl]-6-[(3S)-3-methylmorpholin-4-yl]pyrimidin-2-yl}phenyl)amine (3.6 g, 8.77 mmol) was dissolved in dioxane (20 mL). Sodium bicarbonate (1.1 g, 13.15 mmol) was added, followed by phenyl chloroformate (1.1 mL, 8.77 mmol) and the reaction stirred at room temperature for 2 hours. The solvent was removed in vacuo, and the resultant oil partitioned between 20 mL DCM and 20 mL water. The organic phase was dried over magnesium sulphate, filtered and concentrated in vacuo. The cream solid obtained was chromatographed on silica, eluting with 0-50% ethyl acetate in DCM, to give the desired material as a white solid (2 g).

1. customThe solvent was removed in vacuo
2. customthe resultant oil partitioned between 20 mL DCM and 20 mL water
3. dry with materialThe organic phase was dried over magnesium sulphate
4. filtrationfiltered
5. concentrationconcentrated in vacuo
6. customThe cream solid obtained
7. customwas chromatographed on silica
8. washeluting with 0-50% ethyl acetate in DCM